July / August 2021 NLGI Spokesman

In this issue:…

Serving the Grease Industry Since 1933 - VOL. 85, NO. 3, JULY/AUG. 2021

4 President’s Podium 10 Back to the Basics II: Fundamental Building Blocks of Grease Formulation – The Next Chapter 33 NLGI Annual Meeting September 27-30 | Tuscon, AZ USA 38 High-Performance Multiuse (HPM) Grease Column 41 ASTM D-3527 Retrospective

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PRESIDENT: JIM HUNT Tiarco Chemical 1300 Tiarco Dr Dalton, GA 30720

VICE PRESIDENT: ANOOP KUMAR Chevron Lubricants 100 Chevron Way Room 71-7334 Richmond, CA 94801

SECRETARY: WAYNE MACKWOOD Lanxess Corporation 565 Coronation Dr West Hill, ON, M1E 2K3, Canada PAST-PRES./ADVISORY: JOE KAPERICK Afton Chemical Corporation 500 Spring St Richmond, VA 23218

TREASURER: TOM SCHROEDER AXEL Americas, LLC PO Box 12337 N Kansas City, MO 64116 EXECUTIVE DIRECTOR: CRYSTAL O’HALLORAN, MBA, CAE NLGI International Headquarters 118 N Conistor Ln., Suite B-281 Liberty, MO 64068

SPOKESMAN

NLGI

OFFICERS

Serving the Grease Industry Since 1933 - VOL. 85, NO. 3, JULY/AUG. 2021

4

President’s Podium

6

Industry Calendar of Events

6

Welcome New NLGI Members

6

Advertiser’s Index

DIRECTORS BARBARA A. BELLANTI Battenfeld Grease & Oil Corp of New York PO Box 728 1174 Erie Ave N. Tonawanda, NY 14120 BENNY CAO The Lubrizol Corporation 29400 Lakeland Blvd Mail Drop 051E Wickliffe, OH 44092

DWAINE G. MORRIS Shell Lubricants 526 S Johnson Dr Odessa, MO 64076 JOHN SANDER Lubrication Engineers, Inc. PO Box 16447 Wichita, KS 67216 GEORGE SANDOR Livent Corporation 2801 Yorkmont Rd Suite 300 Charlotte, NC 28208

CHAD CHICHESTER Molykote Lubricants 1801 Larkin Center Drive Midland, MI 48642 CHUCK COE Grease Technology Solutions 35386 Greyfriar Dr Round Hill, VA 20141 MUIBAT GBADAMOSI Calumet Branded Products, LLC One Purple Ln Porter, TX 77365 MAUREEN HUNTER King Industries, Inc. 1 Science Rd Norwalk, CT 06852

SIMONA SHAFTO Koehler Instrument Company, Inc. 85 Corporate Dr Holtsville, NY 11716 JEFF ST. AUBIN AXEL Royal, LLC PO Box 3308 Tulsa, OK 74101 TOM STEIB Italmatch Chemicals 1000 Belt Line St Cleveland, OH 44109 DAVID TURNER CITGO 1293 Eldridge Pkwy Houston, TX 77077

TYLER JARK AOCUSA 8015 Paramount Blvd Pico Rivera, CA 90660

PAT WALSH Texas Refinery Corp One Refinery Pl Ft Worth, TX 76101

STACI SPRINGER Ergon, Inc. PO Box 1639 Jackson, MS 39215 MATTHEW MCGINNIS Daubert Chemical Company 4700 S Central Ave Chicago, IL 60638

RAY ZHANG Vanderbilt Chemicals, LLC 30 Winfield St Norwalk, CT 06855

Jim Hunt, NLGI President

10

Back to the Basics II: Fundamental Building Blocks of Grease Formulation – The Next Chapter Joseph P. Kaperick, Afton Chemical Corporation

33

NLGI Annual Meeting- September 27-30 | Tuscon, AZ USA

38

High-Performance Multiuse (HPM) Grease Column

41

ASTM D-3527 Retrospective

In this issue:…

Serving the Grease Industry Since 1933 - VOL. 85, NO. 3, JULY/AUG. 2021

4 President’s Podium 10 Back to the Basics II: Fundamental Building Blocks of Grease Formulation – The Next Chapter 33 NLGI Annual Meeting September 27-30 | Tuscon, AZ USA 38 High-Performance Multiuse (HPM) Grease Column

Happy Summer!

ON THE COVER

TECHNICAL COMMITTEE CO-CHAIRS ACADEMIC & RESEARCH GRANTS: CHAD CHICHESTER Molykote Lubricants 1801 Larkin Center Drive Midland, MI 48642

EDUCATION: DAVID TURNER CITGO 1293 Eldridge Pkwy Houston, TX 77077

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

TECHNICAL EDITOR: Mary Moon, PhD, MBA Presque Isle Innovations LLC 47 Rickert Drive Yardley, PA 19067

Published bi-monthly by NLGI. (ISSN 0027-6782) CRYSTAL O’HALLORAN, Editor NLGI International Headquarters 118 N Conistor Ln, Suite B-281, Liberty, MO 64068 Phone (816) 524-2500 Web site: http://www.nlgi.org - E-mail: nlgi@nlgi.org The NLGI Spokesman is a complimentary publication.

The current issue can be found on the NLGI website.

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 necessarily represent the official position of NLGI. Copyright 2018, NLGI. Send e-mail corrections to nlgi@nlgi.org.

-3NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

Dear NLGI Family,

Jim Hunt NLGI President 2020 – 2022

We sincerely hope that you and your families are safe and healthy. As you may well know, we are getting closer and closer to our NLGI Annual Meeting planned at the Loews Ventana Canyon, Tucson, AZ September 27-30, 2021. The theme of this year’s annual meeting is “The Future of High-Performance Lubricating Greases.”

We understand there may be some concerns and other dynamics occurring with our NLGI members and meeting attendees that could impact your decision to attend the meeting. Please rest assure the NLGI team is working diligently to provide a successful meeting, including following all local, state and federal safety protocols. The NLGI’s annual meeting success will also dependent upon achieving the highest level of attendees possible. We recognize that many companies may decide to wait to until closer to the meeting date to confirm their intentions to attend the meeting. We truly hope that everyone will attend and register in advance to assist the NLGI team in planning a successful meeting.

As part of our ongoing commitment to continue to keep NLGI members well informed on the status of our six strategic priorities, we will focus this on the High Performance Multiuse (HPM) Certification, including implementation, engagement and marketing.

In December 2020, NLGI launched its High-Performance Grease Multiuse (HPM) Certification and subcategories with enhanced performance. The implementation of the High Performance Multiuse (HPM) Certification has progressed at an unprecedented rate. The level of participation from the grease producers has been outstanding and continues to grow daily. The tremendous efforts from NLGI and the Center for Quality Assurance (CQA) supporting teams, to invest and promote the value of the HPM certification has also had a significant positive impact on future demand for the HPM Certification.

In fact, the NLGI is thrilled to announce the first product approved for the High-Performance Multiuse (HPM) Grease Certification. Castrol’s GR SW 460-1 is the first product certified against the new NLGI HighPerformance Multiuse (HPM) grease specification. In addition, NLGI has certified its enhanced copper corrosion protection, high load carrying capacity and low temperature performance. Tribol GR-SW 460-1 is a specialized product for main bearing applications in wind turbines.

NLGI anticipates a significant increase in NLGI High-Performance Multiuse (HPM) grease specification approvals in the months and years to come. With the assistance of our valued partner, CQA, we will continue to promote the HPM grease certification in future publications, collectively with global grease and lubricant partners and future trade shows to educate and increase the demand for the HPM grease specification certifications in the lubrication industry. We will also provide the highest level of support for all companies requiring assistance in obtaining the HPM certification and/or enhanced sub-categories on their grease.

Additionally, NLGI and CQA will focus marketing efforts on the end-user community. A HPM marketing taskforce was established in January 2021. This taskforce created a robust marketing plan that has been successfully executed over the past several months. These efforts will continue through the remainder of 2021 and into 2022. As of today, NLGI has reached over 622,000 end-users!

Once again, the NLGI is tremendously grateful for your continued support, loyalty, and commitment. We would also want to continue to encourage membership engagement and your attendance at the 2021 Annual Meeting as well as future annual meetings.

The NLGI continues to encourage volunteers for our committees. For more information on volunteer opportunities, please visit HERE. We remain committed to growing our global NLGI membership. If you are interested in becoming a future NLGI member, please contact NLGI HQ at nlgi@nlgi.org or 816-524-2500.

Stay safe and healthy, Jim Hunt President, 2020 – 2022 -4NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

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Industry Calendar of Events 2021 Please contact Denise if there are meetings/conventions you’d like to add to our Industry Calendar, denise@nlgi.org (Your company does not have to be an NLGI membeer to post calendar items.)

NLGI 2021 Annual Meeting

September 27 – 30, 2021

Tucson, AZ, USA

NLGI Annual Meeting

ILMA Annual Meeting

October 9-12, 2021

Phoenix, AZ

ILMA Annual Meeting

2021 Machinery Lubrication October 19-21, 2021 Louisville, KY NORIA Machinery Conference & Exhibition Lubrication Conference

& Exhibition F + L Week Live!

November 15-18, 2021

Bangkok, Thailand

F + L Week Live!

Warm Welcome to our New NLGI Members Gehring-Montgomery Inc.

Biosynthetic Technologies SONGWON Management AG

USA Manufacturer USA Supplier Switzerland Supplier

Advertiser’s Index F&L Asia, page 9 Livent, page 8 The Lubrizol Corporation, page 7 MidContinental Chemical Company, Inc. page 5 NORIA, page 32 Patterson Industries Canada - A Division of ALL-WELD COMPANY LIMITED, page 28 ProSys Servo Filling Systems, page 29 Vanderbilt Chemicals, LLC, Inside Front Cover Zschimmer & Schwarz Inc., page 30

-6NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

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-9NLGI Spokesman ORGANIZED | VOLUME 85,BY NUMBER 3 | July/August 2021

Back to the Basics II: Fundamental Building Blocks of Grease Formulation – The Next Chapter Joseph P. Kaperick Afton Chemical Corporation Richmond, VA, USA

Abstract Earlier work by the author focused on the evaluation of common additives and additive systems in a simple lithium base grease. Some routine and several less common performance tests were used to compare different types of additives and packages and look at the impact of additive combinations.

The focus was on antiwear (AW), extreme pressure (EP), antioxidant (AO) and borate components along with performance packages containing different component combinations.

This study explores the different responses observed in these performance tests when using the above components in a base grease formulated with a lithium complex thickener.

Background Work Previous work by this author investigated the performance of three types of zinc dithiophosphate, two sulfur sources, a combination of antioxidant and boron components aimed at high temperature performance and additive packages formulated to meet various performance targets. The different components were all evaluated in a simple lithium 12-hydroxy stearate grease using a variety of bench tests. The tests ranged from common bench tests included in many specifications to less common evaluations of performance aimed at differentiating characteristics of the additives employed [1].

Much work has been done to evaluate different additive components using a variety of grease bench and rig tests. Some of this work has been published on this subject. Many authors used the Four-Ball Weld test to measure the effectiveness of novel EP agents or in studies of synergies or tribochemical interactions that improve boundary lubrication protection [2-10].

Pressurized Scanning Differential Calorimetry (PDSC) was used by Reyes-Gavilan [11] to evaluate different antioxidants in polyurea- and lithium-thickened greases by a standard test method (ASTM D5483). Senthivel et al. [12] looked at PDSC as well as a variety of other techniques including spectroscopic analysis and thermal aging to investigate the high temperature behavior of greases.

Samman [13] discussed relative characteristics of different components in greases and their relationship to high temperature performance, and he utilized case studies of greases in high temperature applications.

Rheological techniques have become more commonly used in evaluating the performance of high temperature greases in recent years. Nolan and Sivik [14,15] used rheology to compare the high temperature performance of a variety of different thickeners and compared those results to data obtained with a dropping point apparatus. Coe [16] looked at high temperature applications of grease formulations and examined their performance in dropping point as well as a number of other high

- 10 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

temperature bench tests. Kaperick [17] studied the effect of boron additives in lithium greases on performance in the dropping point test.

Rhee [18] used PDSC and a Thermal Gravimetric Analysis (TGA) procedure to build a “decomposition kinetic model” that he correlated to the high temperature wheel bearing rig test (ASTM D3527). Ward and Fish [19] also used PDSC and the D3527 wheel bearing test as a guide and evaluated several finished greases in the FAG FE8 and FE9 rig tests. Additionally, Kaperick [20] investigated tribolayer formation and the effectiveness of different additive systems in various high temperature tests including the FAG FE9 rig test.

Methods and Materials Grease Samples The base grease used for this work was a lithium complex grease that was prepared following the same recipe as the lithium 12-hydroxy stearate greases used in the previous work [1] with the additional step of complexation using azelaic acid as shown in Table 1. This lithium complex base grease was prepared with a blend of paraffinic Group I oils with a KV@40°C of 170 cSt. The alkalinities are reported in %LiOH (not LiOH•H2O) as calculated by ASTM D128, Section 21 – Free Alkali [21].

The base grease was made in the author’s facility using a lab-scale, covered and jacketed 5-gallon kettle operated at atmospheric pressure with a single-motion, anchor-style agitator with scraper blades and fixed vertical baffle attached to the bottom of the lid cover. The heating profiles for both base greases were similar with the exception of the complexation step using azelaic acid, which added approximately 2 hours to the processing time. Heating and cooling were achieved by the circulation of heat transfer oil through the kettle’s jacket using a loop consisting of an oil reservoir, pump, heater, and heat exchanger. The kettle was connected to a second pump that circulated the contents of the kettle through a colloid mill to provide additional agitation and discharged the final product. The operation of the entire unit was computer controlled.

Table 1. Base grease description

For this study, commonly used grease tests were applied to examine the basic responses of a core slate of additives and interactions that might occur in grease formulations. All components were added to the base grease post-production, heated to 60°C for an hour and then thoroughly blended in a centrifugal mixer. These components are shown in Table 2 where some of the physical characteristics (elemental concentrations) are given along with the “IDs” used in various tables and graphs to illustrate the results of the study. Different colors are used for various components for better differentiation in graphs and figures in this paper.

- 11 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

Table 2. Descriptions of components used in this study

The specific types of zinc dithiodiphosphates (ZDDPs) used in the study are shown in Table 3 along with the carbon chain lengths of the primary and secondary alcohols used to make them.

Table 3. ZDDP descriptions

Two types of sulfur compounds were used in the study – a sulfurized isobutylene with a high active sulfur content and a sulfurized olefin with a low active sulfur content. The activity of sulfur was measured using ASTM D1662 and indicated the reactivity of the sulfur componentry with copper.

Details of these two components are shown in Table 4.

Table 4. Sulfur component descriptions

To examine the effect of high temperature componentry on grease formulations, an antioxidant (AO) mixture and a borated dispersant (BPD) were included as detailed in Table 2. These types of components are often used to provide oxidative stability to the oil component (AO) and stability to the thickener at higher temperatures (BPD).

Test Methods The following test methods were employed with variations from standard ASTM methodology noted: • ASTM D2265 “Standard Test Method for Dropping Point of Lubricating Grease Over Wide Temperature Range” [22] - 12 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

• ASTM D2266 “Standard Test Method for Wear Preventive Characteristics of Lubricating Grease (FourBall Method)” [23].

• ASTM D2596 “Standard Test Method for Measurement of Extreme-Pressure Properties of Lubricating Grease (Four-Ball Method)” [24] - This testing was carried out with the modification of using test loads at 10-kg intervals to more accurately monitor the incremental performance of the greases under extreme pressure.

• ASTM D1743 “Standard Test Method for Determining Corrosion Preventive Properties of Lubricating Greases” [25] - According to ASTM D1743, a bearing with no rust spots larger than 1.0 mm in diameter is considered to pass, and two out of three bearings must pass for the grease to be considered acceptable. In the present study, a modified system of rating bearings from D1743 tests was employed to better estimate the impact of each variable on the level of corrosion present. The raceway on the inside of each bearing cup was rated using a visual estimate (without the use of magnification) of the percent surface area covered by rust. This rating method was described in more detail in previous work [26]. To minimize variability in this modification, the same technician did all the evaluations in this study.

• ASTM D6138 “Standard Test Method for Determination of Corrosion-Preventive Properties of Lubricating Greases Under Dynamic Wet Conditions (EMCOR Test)” [27] - Distilled water was used in this study.

• ASTM D 4048 “Standard Test Method for Detection of Copper Corrosion from Lubricating Grease” [28] - Copper strips were immersed in grease samples at the test temperature and removed after the standard 24 h period; then, the strips were rated against the ASTM standard template.

• ASTM D5483 “Standard Test Method for Oxidation Induction Time of Lubricating Greases by Pressure Differential Scanning Calorimetry” [29] - Samples underwent the standard test method at 155°C under a 500 psi (3447 kPa) oxygen atmosphere. The extrapolated onset time was measured and reported as the oxidation induction time (OIT) for each sample.

An Anton-Paar oscillatory rheometer (MCR301) was used to measure the rheological properties of the grease. The grease was compressed between a bottom plate and a parallel top plate. Both plates were 25 mm in diameter and sand-blasted. A hood that contained a temperature-controlled Peltier device was placed over the test grease and bottom plate. A temperature sweep (2°C/min) was performed on the test greases in the rheometer ranging from 40 to 250°C with a constant oscillating shear strain of 0.05%. Both storage modulus (G’) and loss modulus (G”) measurements were taken, and the ratio of the two was plotted as “Tan Delta” (G”/G’). A typical interpretation of this ratio is that as the value increases from less than one to more than one, the internal structure of the grease shifts from a more solid-like material (G’) to a more liquid-like material (G”).

Thermal Gravimetric Analysis (TGA) was completed using a PerkinElmer Pyris 1 instrument. The principle behind TGA involves the measurement of sample weight loss as a function of temperature.

Grease samples were heated from 50°C to 900°C under a nitrogen atmosphere (60 ml/min) using a constant ramp of 20°C/min. The first derivative was plotted, and the rate of weight loss correlated with % weight loss as a function of temperature.

- 13 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

Results and Discussion ZDDP Testing To study differences between the types of ZDDP components, six greases were formulated as shown in Table 5. Due to slight differences in elemental makeup of the different additives, a constant level of phosphorus (640 ppm P) was targeted. A “typical” treat rate of 0.6 wt% of SIB was used to assess the impact of this component on performance of the ZDDPs under various test conditions.

Table 5. ZDDP formulations

Corrosion testing shows some differentiation between these formulations as shown in Table 6. In all steel corrosion testing, the lithium complex base grease provided significantly better protection against rust, even without additives present. In the static rust test (ASTM D1743), the base grease alone showed no rust, so additional testing with ZDDP-containing grease was not carried out. In the more dynamic EMCOR corrosion test (ASTM D6138), the lithium complex base grease was significantly better than the simple lithium base grease with very consistent responses across three duplicate runs. For this test, the presence of ZDDP in the lithium complex base showed consistent improvement regardless of the type of ZDDP, and the presence of SIB appeared to have no impact on that response.

Table 6. ZDDP steel corrosion results

Copper corrosion testing also showed some differences between formulations, Table 7. Again, the lithium complex base grease showed better response than the lithium base grease; two out of three runs had 1b ratings for the lithium complex base grease. Due to this good response, it’s difficult to tell if the addition of ZDDP was helpful for the copper corrosion performance of the lithium complex base grease as was indicated for the simple lithium base. The addition of SIB did result in some improvement of copper corrosion performance across the ZDDP types, although it was difficult to distinguish between the ZDDP types. This result was similar to what was seen in the simple lithium greases but appeared to be more exaggerated in the lithium complex.

- 14 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

Table 7. ZDDP copper corrosion results

PDSC was used to compare the properties of ZDDP as a secondary antioxidant in both lithium and lithium complex greases. The values for the simple lithium greases were originally obtained at 155⁰C, while it was decided to use the more appropriate temperature of 180⁰C for the additional work in the lithium complex greases (see Figure 1). Therefore, the simple lithium PDSC data was converted using a common equation (Eq. 1) based on the Arrhenius relationship.

OIT(180⁰C) = OIT(155⁰C) /(2^2.5)

(1)

This equation assumes that the oxidative life of a grease is reduced by half for every 10⁰C rise in temperature, with “2^2.5” being the adjustment needed with a change in temperature of 25⁰C. Under the conditions of the PDSC test, very little difference was seen between the two different thickener systems, with all the formulations containing ZDDP having a positive impact with increasing oxidation induction times (OIT). The expected relationship between the types of ZDDP was maintained with secondary ZDDP showing the best stability. The addition of SIB appeared to have more of a negative impact on the lithium complex formulation, which may correlate with the same phenomenon that we saw in copper corrosion due to interactions within the complex structure.

Figure 1. ZDDP oxidation (PDSC) results - 15 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

To further examine the impact of ZDDP on the thermal stability of grease formulations, TGA testing was used. Since this technique is not commonly used for analysis of greases, in this study, the base grease was tested followed by duplicate runs of a fully formulated grease to evaluate repeatability. As shown in Figure 2, the base grease had two main components that were separated by their thermal stability under the conditions of the test. The majority of the grease sample (the base oil component) burned off between 200 and 430⁰C, while the thickener , which was more thermally stable, was removed between 440 and 600⁰C. The repeatability of the technique was seen with duplicate runs of a representative sample “B”.

Figure 2. Base grease response and repeatability of TGA data

The differences in thermal stability between the simple and complex lithium thickeners (Figure 3) are immediately obvious and very unlike the lack of differentiation seen in the oxidative stability as measured by PDSC. It is worth noting that the TGA analysis was run in a nitrogen atmosphere and monitored weight loss as temperature was increased; therefore, TGA was more a measure of the stability of the grease structure itself, as opposed to the PDSC analysis, which was carried out under oxygen and measured the oxidative stability of the mixture. Here the lithium complex base grease demonstrated much better thermal stability than the simple lithium base grease; the bulk of the mass of the lithium complex base grease (likely the base oil) coming out at 450⁰C almost 100⁰C higher than in the simple lithium base grease. Some similar features such as small peaks seen around 370-380⁰C and at 460-470⁰C may indicate some structures common to both greases.

- 16 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

Figure 3. Comparison of TGA data for simple and complex lithium base greases

The impact of the addition of different types of ZDDP to the lithium complex base grease stability is seen in Figure 4. In general, there is some indication of improved thermal stability in both base greases but no real differentiation between types such as was seen with oxidative stability. These improvements can be seen particularly on the right side of the peaks where the addition of ZDDP consistently increases thermal stability by 10 to 20⁰C. This effect is likely due to some additional structural stability from crosslinking between the ZDDP and soap structure, but additional study is needed to better understand how these data relate to grease structure and the impact of additives.

Figure 4. ZDDP thermal stability (TGA) data - 17 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

Another way to look at thermal stability of the grease structure, high temperature rheology, has been used more in recent research. By monitoring the ratio of G” and G’ while gradually raising the temperature, the impact of temperature on grease behavior can be closely observed. This ratio is typically referred to as “Tan Delta”. It characterizes the shift of the grease sample from more solid-like behavior at low Tan Delta values to more liquid-like behavior at higher values, which is commonly seen with increasing temperature. The temperature at which there is an abrupt rise in Tan Delta can be roughly correlated to the dropping point, but Tan Delta can also provide significantly more information about the high temperature performance of greases.

In the original analysis of the simple lithium base grease, as seen in Figure 5, the rise in temperature led to an initial slight “solidification” of the grease structure starting at around 60⁰C, followed by a gradual change to a more liquid-like phase from 100⁰C to approximately 190⁰C. This was followed by a sharp increase in Tan Delta that correlated roughly to the 205⁰C dropping point seen with this base grease. As the temperature continued to increase, the signal deteriorated rapidly as the oil ran out of the grease, and consistent contact between the plates was lost. The repeatability of the method was quite good as shown by the two runs overlaid on top of each other.

The lithium complex base grease showed distinct differences in this testing with markedly different response than the simple lithium grease. In the range around 200⁰C (at which temperature the simple lithium base grease lost structure), the lithium complex base grease underwent a small change in structure before it returned to its previous level of Tan Delta between 0.2 and 0.3 (see Figure 6). The response was also different in that the dropping point for the lithium complex base was 283⁰C, but there was no indication of structural loss at that temperature in the rheology scan.

Figure 5. Base grease response in high temperature rheology

- 18 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

The obvious impact of ZDDP addition for both greases was to increase the structural stability as seen in Figure 7. This was more apparent in the lithium base grease at the dropping point (203⁰C), but in the lithium complex there was a more subtle “leveling” effect seen in the increase in Tan Delta between 90⁰C and 160⁰C and the reduction in Tan Delta between 200⁰C and 220⁰C. The overall impact appears to be that ZDDP helped maintain a consistent structure of the lithium complex base in a manner similar (although different in specific aspects) to that seen in the simple lithium base. And while there may be some differences between the responses of ZDDP types at medium and very high temperatures, additional work would be needed to determine their significance.

Figure 6. Comparison of base grease types (rheology)

Figure 7. ZDDP response in high temperature rheology - 19 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

ZDDP is often used as a primary antiwear component in grease formulations, so the impact on the commonly used Four-Ball Weld and Wear tests was evaluated. As seen in Figure 8, there was a small increase in the weld load of the lithium complex base over the simple lithium, which was even greater with the addition of ZDDP. The addition of SIB, as expected, increased the weld loads even higher, but there was no indication of a variation of response between different ZDDP types. In all cases, the lithium complex base grease gave a better weld load than that seen with the simple lithium base.

Figure 8. ZDDP extreme pressure

In the evaluation of the antiwear properties using the Four-Ball Wear Test, an increase in wear protection was seen in the lithium complex base grease as well as five out of the six greases formulated with ZDDP and SIB combinations (see Figure 9). While none of the differences were statistically significant within the repeatability of ASTM D2266, the trend toward lower wear in the lithium complex base grease seems apparent. As with the weld load testing, no significant differences (or trends) were noted between different ZDDP types.

Figure 9. ZDDP wear testing - 20 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

Sulfur Testing The two sulfur sources were blended into four formulations to investigate the impact of the sulfur component, alone and in the presence of the primary ZDDP (Table 8). Due to the wide disparity in sulfur content, the level of each sulfur component was calculated to target an equivalent level of sulfur (2780 ppm) in each formulation. The level of ZDDP was kept the same as in the study of the ZDDP components above.

Table 8. Formulations for sulfur study

In all steel corrosion testing, the presence of the SIB surprisingly diminished the corrosion prevention properties of the lithium complex base grease (Table 9). While it was a mild impact, it was in contrast to the improvement seen with sulfurized olefin that reduced the EMCOR ratings to the same level (1/1) as the ZDDP components. This was also different from the simple lithium base, which showed only a positive impact from either sulfur source. Of interest is that the addition of ZDDP negated the impact of the SIB and brought it to the same level as the sulfurized olefin or ZDDP by itself. This contrasted with the simple lithium base grease, which showed indications of a negative impact from the interaction of sulfur and ZDDP. Further study would be needed to confirm these initial indications.

Table 9. Sulfur steel corrosion results

Variability in copper corrosion testing led to the need to repeat several observations, but the results (Table 10) seem to indicate better copper corrosion protection from the lithium complex base as compared to the simple lithium base grease. It is clear that both types of sulfur caused copper corrosion in the lithium complex grease. This was different from the performance of the sulfurized olefin in the simple lithium where no negative impact was observed. The negative results of SO in lithium complex were surprising due to its low active sulfur content and its previously shown behavior in simple lithium base. Along with other results seen in this study, this may indicate some interactions within the structure of the lithium complex grease that were not seen in the simple lithium grease. Further evidence of this might be the positive impact of the addition of ZDDP, which may interact with the sulfur to eliminate its negative effect.

- 21 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

Table 10. Sulfur copper corrosion results

Sulfurized olefin is used as an antioxidant in engine oils and other formulations, so it was not surprising to see that it provided oxidative stability to the simple lithium base grease. However, a similar impact was not seen in the lithium complex grease in which both sulfur types seemed to give less improvement in oxidative stability as measured by PDSC (Figure 10). The addition of ZDDP gave a boost to both sulfur types, but the overall improvement was not as great as that seen in the simple lithium base grease, and there was less differentiation between the two sulfur sources.

Since sulfur is often used primarily for extreme pressure protection, testing was done for Four-Ball Weld (Figure 11). As discussed earlier, the lithium complex base grease showed better weld loads, the addition of sulfur boosted the base grease response by about the same amount, and the difference between the sulfur types was less distinct than it was in the simple lithium grease. The addition of the ZDDP seemed to have the opposite effect by boosting the SIB-containing formulation more than the SO formulation and leading to a larger discrepancy between the two.

Figure 10. Sulfur oxidation results

- 22 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

Figure 11. Sulfur weld load results

Finally, the sulfur-containing formulations were evaluated for wear protection using Four-Ball Wear testing (Figure 12). The inherent wear reduction seen for the lithium complex base grease was even more dramatic with both sulfur types. While the addition of either sulfur source in the simple lithium grease led to very high wear levels, in the lithium complex base, they showed a reduction that if not statistically significant, at least trended in the opposite direction. The addition of ZDDP seemed to further contribute to this reduction in wear and, again, to a higher degree than in the simple lithium grease.

Figure 12. Sulfur wear protection results

- 23 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

Antioxidant/Borate Testing A third category of additives was tested in the initial study because of its importance for the high temperature performance for many greases. Antioxidants are considered useful for enhancing the oxidative stability of the base oil (the major component of grease formulations) under high temperature or other conditions of thermal-oxidative stress. Borated components are also widely considered useful for improving high temperature performance due to their ability to strengthen the grease thickener structure at high temperatures as measured by dropping point. Additionally, borates are thought to work synergistically with ZDDP. For this reason, ZDDP was included with the antioxidant mixture, and borate (BPD) was added sequentially. Two levels of the borate were examined in combination with the ZDDP and the AO mixture (Table 11).

Table 11. Antioxidant/borate formulations

As expected, the lithium complex base gave a much higher dropping point than the simple lithium base grease, and the addition of AO and ZDDP had little impact on either base grease (Table 12). The addition of a lower level of the borate raised the dropping point of the complex grease, but the higher treat level appeared to disrupt the complex structure in some manner, leading to a lower dropping point than observed for the simple lithium grease with the same amount of borate. This is another example of some level of interaction between additives and the complex soap structure that would benefit from additional study.

Table 12. AO/Borate dropping point results

Minimal testing was done with copper corrosion due to the expectation that these components were unlikely to significantly affect performance. However, EMCOR corrosion testing (Table 13) gave somewhat surprising results. In the lithium base, an unexpected improvement was seen with the addition of AO and BPD, possibly due to the aminic portion of the AO componentry or the reaction of the borated species with the water, keeping it away from the steel surface. The lithium complex formulation showed the same improvement with the addition of ZDDP (as in the simple lithium base), but that impact was reduced by the addition of AO and resulted in higher EMCOR ratings in duplicate runs. Even more surprising were the ratings obtained after the addition of the BPD. The 1.5 wt% BPD treat resulted in a wide spread of results across four different duplicate runs. The 3 wt% BPD treat showed much more repeatable results that were very similar to those with only the ZDDP added.

This may be further indication of interactions between structure and different componentry that has positive and negative impacts on performance in various bench tests. Further study would be needed to confirm the mechanism.

- 24 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

Table 13. AO/Borate steel corrosion results

As expected in oxidation testing by PDSC (Figure 13), the addition of the AO mixture had an incremental benefit when used in combination with the ZDDP, which provided some oxidation stability itself. However, as seen previously with the ZDDP testing, the lithium complex greases lagged behind the simple lithium formulations. The addition of the higher treat of BPD had a significant impact on the OIT, which was not seen in the simple lithium base grease. An additional sample without ZDDP showed only an incremental benefit with this component and not a synergistic effect, such as that associated with the use of boron to raise the dropping point.

Testing by TGA showed definite evidence of increased thermal stability of the lithium complex formulations compared to simple lithium, as discussed above (Figure 14). There was evidence of slight increases in thermal stability with the addition of the BPD (especially with the pronounced peak at around 500⁰C) and the slight decrease in thermal stability seen in the formulation with no ZDDP. This is not unexpected and the lack of improvement (such as seen with the addition of the BPD to the simple lithium base) may indicate that some kind of maximum thermal stability has been reached.

High temperature rheology of these greases also highlighted the different response to high temperature by the simple lithium and lithium complex grease formulations. As seen in Figure 15, the addition of the ZDDP and AO to the simple lithium resulted in a restabilization of the signal around 230⁰C after a sharp disruption around 200⁰C (at which temperature this formulation still experienced a dropping point). However, the addition of the BPD almost completely removed that disruption, although the liquid-like nature of the sample continued to increase as the sample was heated to 300⁰C.

Figure 13. AO/Borate oxidation results - 25 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

It is also worth noting that the dropping points of these samples changed significantly with the addition of the BPD as seen in Table 13. In the lithium complex base grease (Figure 16), the loss of signal disruption was previously noted and corresponded to the much higher dropping point. The addition of the ZDDP and AO showed a significant increase in liquid-like behavior of the grease between 110⁰C and 140⁰C, which was negated by the addition of the BPD and not seen without the ZDDP. At higher temperatures, there was clear evidence that the BPD added some liquid-like nature to the sample.

Figure 14. AO/Borate TGA results

The higher level seemed to push that liquid-like nature to a higher temperature. This may indicate some interaction between the complex thickener and the borated component. In all cases, the Tan Delta response was lower for the lithium complex greases, indicating a more thermally stable configuration, versus the simple lithium greases. Further work at these higher temperatures would be of interest as well.

- 26 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

Figure 15. AO/Borate high temperature rheology results - lithium

Figure 16. AO/Borate high temperature rheology results – lithium complex

- 27 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

Summary and Conclusions In general, the lithium complex base grease showed better performance than the simple lithium base grease in the reduction of steel corrosion, additional protection against wear and extreme pressure,

and thermal stability. The thermal stability increase was seen in the dropping point, TGA data and better maintenance of structure in high temperature rheology testing. This improvement in thermal stability was not accompanied by an increase

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in oxidative stability, and the response in the copper corrosion tests seemed similar for both thickener systems.

ZDDP – ZDDP is typically used in grease as an antiwear agent that can also provide some benefits as a secondary antioxidant through its role as a peroxide decomposer. In this study, the ZDDP significantly boosted the performance of the lithium complex greases in the EP and AW tests; this improvement was better for the lithium complex than simple lithium greases, probably due to the performance of the unadditized base greases. In PDSC oxidation testing, the greases with the ZDDP showed good improvement over the base greases, but the lithium complex greases did not outperform the lithium greases.

Protection was seen in both steel and copper corrosion tests, and evidence was also observed for stabilization of the grease thickener structure at higher temperatures in both the TGA and high temperature rheology measurements, with the lithium complex formulations showing better performance than the simple lithium formulations in all these areas. There did not seem to be any indication of different responses due to the type of ZDDP except in the case of oxidation testing, in which the order of stability was predictable: secondary>mixed>primary.

Sulfur – The role of sulfur

- 28 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

in protecting surfaces under extreme pressure was confirmed, but the normal decrease in wear protection was not seen in the lithium complex formulations. While both sulfur sources provided some additional protection against steel and copper corrosion in the simple lithium greases, in the lithium complex greases the SIB worsened both steel and copper corrosion, and the SO gave a similarly poor response in copper corrosion testing. This was unexpected due to the lower activity of the sulfur in the SO. In both cases, the ZDDP seemed to negate the poor response, possibly due to interaction with the sulfur species and/or the complex thickener itself. The sulfurized olefin also helped reduce steel corrosion by itself and provided some oxidation benefits, but not to the extent seen in the simple lithium grease. In the PDSC testing, the addition of the ZDDP again raised the performance level of both sulfur types, but differentiation between the two types was less distinct.

These interactions need to be considered when formulating with both component types.

AO/Borate – While the dropping point of the lithium complex base grease was expectedly much higher than that of the simple lithium base grease, the addition of the BPD at higher levels seemed to have an effect on the complex structure as seen in a lowering of the dropping point. This

may be related to the atypical behavior seen in the EMCOR corrosion testing in which the ZDDP and AO improved ratings, but a moderate treat (1.5 wt%) of the BPD resulted in wide variation in corrosion protection that might indicate

Servo Filling Systems

some complex interactions between the BPD, lithium complex soap structure and other components present. In oxidation testing, the expected benefit of the AO was obtained along with a small additional benefit of the high treat (3

EST. 1985

- 29 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

wt%) of BPD, which was not anticipated. Finally, the benefits of the BPD, AO and ZDDP componentry in improving thermal stability were observed in both TGA and high temperature rheology testing.

These benefits were in addition to the already improved

stability of the lithium complex base grease compared to the lithium base grease.

Future – Additional work is needed in many areas that were examined in both of these studies of lithium-thickened greases. The high temperature

work with TGA and rheology continued to show interesting differences that can be linked to additive componentry, but this area needs further study to correlate these findings to bearing response at high temperatures. Finally, it would be of interest to look further at some of the unexpected results that might indicate more complex interactions between thickener structure and additive components in several performance areas.

References

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[1] Kaperick, J: “Back to the Basics - The ABC’s of Grease Additive Performance,” NLGI Spokesman, 84 (2020) 2, 27-53.

[2] Scott, William P., “Extreme Pressure Lubricants,” U.S. Patent 3,133,020, (1964).

[3] Collins, Albert V., “Lubricant Compositions Containing Zirconyl Soaps,” U.S. Patent 4,171,268, (1979).

[4] Mobil Research, “Gear Lube Test predicts performance,” Engineering, 212, p. 1085, (Nov. 1972).

[5] Fang, X.; Liu, W.; Qiao, Y.; Xue, Q. and Dang, H., “Industrial gear oil – a study of the interaction of antiwear and extreme-pressure additives,” Tribology International, 26, pp. 395-8, (1993).

[6] Kubo, K.; Shimakawa, Y. and Kibukawa, M., “Study on the Load Carrying Mechanism of Sulphur-Phosphorus Type Lubricants,” Proceedings of the JSLE International Tribology Conference, 3, pp. 661-6, (1985).

[7] Feher, J.J. and Malone, B.W., “The evolution of EP additives for greases and industrial gear lubricants,” NLGI Spokesman, 52, pp. 553-8, (1989).

- 30 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

[8] Hein, Richard W., “Evaluation of Bismuth Naphthenate as an EP Additive,” Journal of the Society of Tribologists and Lubrication Engineers, pp. 45-51, (November, 2000).

[9] Ward, William C. and Najman, Morey, “Properties of Tribochemical Films from Various Additives in Grease Generated under Load,” Presented at the 72nd Annual Meeting of the NLGI, at San Antonio, Texas, (2005).

[10] Fu, X.; Shao, H.; Ren, T.; Liu, W. and Xue, Q., “Tribological characteristics of di(iso-butyl) polysulfide as extreme pressure additive in some mineral base oils,” Industrial Lubrication and Tribology, 58, pp. 145-150, (2006).

[11] Reyes-Gavilan, J.; Hamblin, P.C.; Laemlin, S.; Rohrbach, P.; Zschech, D.: “Evaluation of the Thermo-Oxidative Characteristics of Greases by Pressurized Differential Scanning Calorimetry,” NLGI 70th Annual Meeting, October 2003, Hilton Head, South Carolina, USA. [12] Senthivel P; Joseph, M.; Nagar S.C.; Kumar, A.; Naithani, K. P.; Mehta, A. K.; Raje, N.R.: “An Investigations Into the Thermal Behaviour of Lubricating Greases

by Diverse Techniques,” NLGI 71st Annual Meeting, October 31 – November 2, 2004, Dana Point, California, USA. [13] Samman, N.: “High Temperature Greases,” NLGI Spokesman, 70 (2007) 11, pp. 1423.

[14] Nolan, S.J; Sivik, M.R.: “The use of controlled stress rheology to study the high temperature structural properties of lubricating greases,” NLGI Spokesman, 69 (2005) 4, 14-23.

[15] Nolan, S.J; Sivik, M.R.: “Studies on the High-Temperature Rheology of Lithium Complex Greases,” NLGI 74th Annual Meeting, June 10-12, 2007, Phoenix, Arizona, USA. [16] Coe, C: “Shouldn’t Grease

Upper Operating Temperature Claims Have a Technical Basis?”

NLGI Spokesman, 72 (2009) 10, 20-28.

[17] Kaperick, J; Aguilar, G; Garelick, K; Miller, A; Lennon, M; Edwards, M: “Complex Issue of Dropping Point Enhancement in Grease,” NLGI Spokesman, 81 (2017) 5, 36-47.

[18] Rhee, I: “Prediction of High Temperature Grease Life Using a Decomposition Kinetic Model,” NLGI Spokesman, 74 (2010) 2, 28-35.

[19] Ward, W. Jr.; Fish, G.: “Development of Greases with Extended Grease and Bearing Life Using Pressure Differential Scanning Calorimetry and Wheel Bearing Life Testing,” NLGI 76th Annual Meeting, June 13-16, 2009, Tucson, Arizona, USA. [20] Kaperick, J.: “If You Can’t Stand the Heat...The Effects of Temperature on Grease Additive Performance,” NLGI 78th Annual Meeting, June 11-14, 2011, Desert Springs, CA, USA. [21] ASTM D128 “Standard Test Methods for Analysis of Lubricating Grease”, Section 21 – Free Alkalinity, ASTM International, West Conshohocken, PA. [22] ASTM D2265-15e1 “Standard Test Method for Dropping Point of Lubricating Grease Over Wide Temperature Range”, (2015) ASTM International, West Conshohocken, PA. [23] ASTM D2266-01(2015) “Standard Test Method for Wear Preventive Characteristics of Lubricating Grease (FourBall Method)”, (2015) ASTM International, West Conshohocken, PA. [24] ASTM D2596-15 “Standard Test Method for Measurement of Extreme-Pressure Properties of Lubricating Grease (FourBall Method)”, (2015) ASTM International, West Conshohocken, PA.

[25] ASTM D1743-13(2018) “Standard Test Method for Determining Corrosion Preventive Properties of Lubricating Greases”, (2018) ASTM International, West Conshohocken, PA. [26] Kaperick, J.P., Rust for the Record: Significant Factors Affecting Corrosion Protection in Grease, NLGI Spokesman, 82 (2018) 3, 34-45.

[27] ASTM D6138-18 “Standard Test Method for Determination of Corrosion-Preventive Properties of Lubricating Greases Under Dynamic Wet Conditions (EMCOR Test)” (2018)ASTM International, West Conshohocken, PA. [28] ASTM D4048-16e1 “Standard Test Method for Detection of Copper Corrosion from Lubricating Grease”, (2016) ASTM International, West Conshohocken, PA. [29] ASTM D5483-05(2015) “Standard Test Method for Oxidation Induction Time of Lubricating Greases by Pressure Differential Scanning Calorimetry”, (2015) ASTM International, West Conshohocken, PA.

Acknowledgements Many thanks for valuable work carried out by the following colleagues at Afton Chemical Corporation: Mike Lennon, Brandi Ford, Mike Jennings, Cody Walker, Zach Adams, Anna Wright, Karen Hux and Dirk Burmeister.

This paper was presented as #2020-08 at the NLGI 87th Annual Meeting, held virtually on August 27, 2020.

- 31 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

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NLGI 2021 ANNUAL MEETING September 27-30 | Tuscon, AZ USA

• SCHEDULE OF EVENTS • MONDAY, SEPTEMBER 27, 2021 7 AM - 12 PM 12 PM - 2 PM 12 PM - 5:30 PM 2:30 PM - 4:30 PM 5 PM - 6 PM 6 PM - 7 PM

Table-Top Exhibits Setup................................................................. Grand Ballroom Executive Committee Meeting with Lunch...............................................Coronado Registration & Exhibits Open.......................................................... Grand Ballroom Board of Directors Meeting...................................................Ventana Dining Room New Member/First-Timer Reception (Invitation Only)......................Upper Terrace Welcome Reception................................................... Bill’s Grill & Cascade Terrace

TUESDAY, SEPTEMBER 28, 2021 6:45 AM - 7:45 AM 8 AM - 12:30 PM 8 AM - 5:15 PM 8 AM - 5 PM 10AM - 5PM 1 PM - 5 PM 1 PM - 2 PM 2 PM - 3 PM 3 PM - 4 PM 4 PM - 5 PM 5:15 PM - 6:15 PM 6:15 PM - 6:30 PM 6:30 PM - 8 PM

Golfer’s Breakfast........................................................................................Flying V Golf Tournament - Shotgun Start*...............................................Mountain Course Basic Lubricating Grease Course*.......................................... Executive Boardroom Advanced Lubricating Grease Course*................................Hospitality Parlor 2205 Registration & Exhibits Open.......................................................... Grand Ballroom Working Group Meetings ...........................................................Catalina Ballroom • Food Grade • Grease Specifications • Grease Particle • Biobased Opening General Session................................................................... Kiva Ballroom Award Winner Photo Session............................................................ Kiva Ballroom Networking Reception............................................................................. Kiva Patio

WEDNESDAY, SEPTEMBER 29, 2021

7 AM 7 AM - 4 PM 7:30 AM - 8:45 AM 8:45 AM - 10 AM 10:30 AM - 11:55 AM 10 AM - 12 PM 12 PM - 1 PM 1 PM - 5:45 PM 1 PM - 4:15 PM 1 PM - 4 PM 2:45 PM - 3:30 PM

Fun Run* - Complimentary Event.............................................................. Par Course Registration & Exhibits Open.......................................................... Grand Ballroom Networking Breakfast..................................................................... Grand Ballroom Industry Speaker................................................................................ Kiva Ballroom Technical Presentations - Session 1.............................................Catalina Ballroom Spouse/Guest Activity*............................................................................Coronado Networking Lunch.......................................................................... Grand Ballroom Technical Presentations - Session 2.............................................Catalina Ballroom Basic Lubricating Grease Course*.......................................... Executive Boardroom Advanced Lubricating Grease Course*................................Hospitality Parlor 2205 Snack Break.................................................................................... Grand Ballroom

THURSDAY, SEPTEMBER 30, 2021

7 AM - 7:45 AM 7 AM - 8:30 AM 7 AM - 3 PM 8:45 AM - 12 PM 12 PM - 1:30 PM 1:45 PM - 5 PM 2 PM - 4 PM 3 PM - 5 PM 3 PM - 3:30 PM 6 PM - 9 PM

Networking Breakfast..................................................................... Grand Ballroom Board of Directors Meeting with Breakfast...........................Ventana Dining Room Registration & Exhibits Open.......................................................... Grand Ballroom Technical Presentations - Session 3.............................................Catalina Ballroom Networking Lunch.......................................................................... Grand Ballroom Technical Presentations - Session 4.............................................Catalina Ballroom CLGS Exam................................................................................................Coronado Table Top Exhibits Teardown.......................................................... Grand Ballroom Snack Break.......................................................................... Grand Ballroom Foyer Closing Night Celebration & Dinner....................................................Coyote Corral

* Optional event, Fee-based, Registration required

https://www.nlgi.org/annual-meeting/2021-annual-meeting/schedule-program/ - 33 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

INDUSTRY SPEAKER Selda Gunsel

Wednesday, September 29 8:45 AM - 10:00 AM

Presentation Topics Include: • Trends in the industry • Case for a sustainable future for the world and the industry • Shell’s sustainability objectives • Role of technology and innovation on this journey • What high-performance greases can do now and into the future Selda Gunsel is the Vice President of Global Commercial and Fuels Technology within Shell’s Projects & Technology organisation with responsibility for leading a global group of scientists and engineers in the delivery of innovation, R&D and technical services to Shell Lubricants, Retail and B2B businesses including Marine, Aviation, and Specialties. Selda is based in Houston, USA. Selda was elected to the National Academy of Engineering in the USA in 2017 in recognition of her distinguished contributions to engineering, “for leadership in developing and manufacturing advanced fuels and lubricants to meet growing global energy demand while reducing CO2 emissions”. Election to the National Academy of Engineering is among the highest professional distinctions accorded to an engineer.

In 2015, Selda was awarded the STLE International Award – the highest technical honor awarded by the Society of Tribologists and Lubrication Engineers. Throughout her career, Selda has received numerous other awards including STLE Fellow for outstanding personal achievement in lubrication science, R&D 100 Innovation Award, SAE International Excellence in Presentation Award, STLE Captain Alfred E. Hunt Best Paper Award, Penn State Outstanding Engineering Alumna Award and internal awards for both Innovation and Leadership in Diversity and Inclusiveness.

In January 2013, Selda was appointed as an Honorary Professor at Beijing’s Tsinghua University with whom Shell enjoys a partnership to deepen the understanding of lubricants. This coincided with Selda being based in Shanghai from 2012-2014 to oversee the development and launch of a new Shell Lubricants Technical Centre to serve the Asian market.

Before joining Shell in 2002, Selda was the Vice President of Technology Development and Innovations at Pennzoil-Quaker State Company. Subsequently, Selda’s roles in Shell have included Vice President of Fuels and Engine Vehicle Technology; General Manager of Global Products & Quality; General Manager of Lubricants Technology Americas; and General Manager of Global Lubricants Strategic R&D. Selda received her BSc in Chemical Engineering from the Istanbul Technical University in Turkey and her MSc and PhD also in Chemical Engineering from the Pennsylvania State University, USA. While working in the industry, Selda has held sabbatical assignments at Imperial College, London in the UK. Selda has published extensively in the field of lubrication science, received patents and is well known in the industry. She has served as the President of the STLE and the Chairman of the Society of Automotive Engineers (SAE) Lubricants Research Award Board. She is a member of the Industrial Advisory Board of Penn State University and has served on the Editorial Boards of the Journal of Lubrication Science, UK, and Tribology Transactions, USA. She has chaired and delivered keynote addresses at many international conferences.

For more information visit: https://www.nlgi.org/annual-meeting/2021-annual-meeting/industry-speaker/ - 34 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

• TECHNICAL SESSIONS 1 & 2 •

WEDNESDAY, SEPT 29 SESSION 1 - 10:30 AM - 11:55 AM 10:30 AM-11:10 AM

2117

2020 Grease Production Survey

Chuck Coe Grease Technology Solutions

11:15 AM-11:55 AM

2103

Regulatory Compliant PTFE Powders for Grease Applications

Shichiu Kwan Shamrock Technologies

12:00 PM-1:00 PM

NETWORKING LUNCH

SESSION 2- 1:05 PM - 5:40 PM 1:05 PM-1:45 PM

2115

Tribochemistry and Tribological Performance of Advanced Parash Kalita Bearing Grease Fortfied with Novel Self-Assembled VinTech Nano Materials Nanocarbon Additives

1:50 PM-2:30 PM

2102

A Comparative Study of Greases Manufactured Using Microwaves with Greases Manufactured Using Conventional Heat Transfer Oil Heating

2:35 PM-3:15 PM

2101

3:15 PM-3:30 PM

Lou Honary Environmental Lubricants Manufacturing (ELM) Anoop Kumar* Chevron Lubricants

An Experimental Study of the correlation Between Low Temperature Mobility, Tackiness, and Water Resistance In a Variety of Greases

Raj Shah Koehler Instrument Company

BREAK Alan Gurt* Louisiana State University

3:30 PM-4:10 PM

2118

Reliably Testing Grease Consistency with Small Samples

4:15 PM-4:55 PM

2110

Novel Lithium Free Thickener System: Performance Profile, Characteristics and Target Applications

Dwaine Morris Shell

5:00 PM-5:40 PM

2114

Grease R-evolution 2021

George Dodos ELDON’S SA

Michael Khonsari Louisiana State University

*Denotes Presenter

- 35 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

• TECHNICAL SESSION 3 • THURSDAY, SEPT 30 SESSION 3 8:45 AM - 11:55 AM 8:45 AM - 9:25 AM

2108

Modified Fatty Acids As Alternative Soap Thickeners for Lubricating Greases

Devin Granger* Ingevity Shadaab Maghrabi Ingevity Juan Bosch Giner* University of Akron

9:30 AM -10:10 AM

2116

Christian Ondarza University of Akron

2020 Research Grant

Barbara Fowler University of Akron Gary Doll University of Akron

10:10 AM-10:25 AM

10:30 AM - 11:10 AM

11:15 AM - 11:55 AM

BREAK

2112

2104

Covering the Bases - A Study of the Influence of Synthetic Base Fluids on High Performance Greases

Effect of Temperature, Surface Roughness and Material on the Tribological Behavior of Electric Motor Greases as a Baseline for Electric Vehicle Bearing Applications

12:00 PM - 1:30 PM

Joe Kaperick* Afton Chemical Corp Luca Salvi ExxonMobil Chemical Dr. Ashlie Martini* Univ of CA, Merced Samuel Leventini Univ of CA, Merced Daniel Sanchez Garrido Univ of CA, Merced

NETWORKING LUNCH

• TECHNICAL SESSION 4 • THURSDAY, SEPT 30 SESSION 4 1:45 PM - 3:10 PM 1:45 PM- 2:25 PM

2:30 PM -3:10 PM

2107

Overcoming Obstacles in Water Resistant H1 and Biobased Specialty Greases Using Polymer

2119

Innovations in High Performance, Environmentally Acceptable Lubricants (EALs) in Grease Application: A Real World Perspective

Erik Willett Functional Products Mark Miller* Biosynthetic Technologies Matt Kriech Biosynthetic Technologies *Denotes Presenter

- 36 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

BASIC LUBRICATING GREASE COURSE Tuesday, September 28 from 8 AM - 5:15 PM Wednesday, September 29 from 1 PM - 4:15 PM Offered once per year during the NLGI Annual Meeting, this in person course is a great way to obtain additional knowledge about the industry, prep for the Certified Lubricating Grease Specialist (CLGS) exam and more.

With more than a 1200 alumni, NLGI’s Basic Lubricating Grease Course is the world’s foremost foundational training class for the global grease industry. This course provides an excellent overview of the types of greases, thickeners, base oils and additives. The methods of manufacturing, testing methodology and their use in bearings and in industrial and automotive applications are also covered. Topics include the following: • Introduction to Greases • Grease Testing • Base Oils • Grease Selection and Recommendations • Performance Additives • Industrial Applications • Grease Manufacturing • Automotive Applications • Grease Packages and Dispensing • Trouble Shooting

ADVANCED LUBRICATING GREASE COURSE Tuesday, September 28 from 8 AM - 5 PM Wednesday, September 29 from 1 PM - 4 PM Offered once per year during the NLGI Annual Meeting, this in person course is a great way to obtain additional knowledge about the industry, prep for the Certified Lubricating Grease Specialist (CLGS) exam and more.

This course provides advanced instruction regarding specific types of greases, grease chemistry and specialized applications. There is an increased focus on high-value specialty greases and their manufacture and use. Topics include the following: • Special Tests • Steel Mill Greases and Other Lubricants • Soap Manufacturing • Applications: Problems • Polyurea Greases • Solid Additives • Applications: Grease Tribology • Silicone Greases • Bearing Lubrication Greases & Gear Oils • Calcium Sulfonate Greases • Food Grade Lubricants • Synthetic Lubricants Base Stocks

CERTIFIED LUBRICATING GREASE SPECIALIST (CLGS) Thursday, September 30 from 2 PM - 4 PM

A standard that certifies that an individual possesses a defined level of expertise in the field of lubricating grease.

Certification indicates that NLGI recognizes the individual as a grease expert. Certification is awarded after an individual passes a two-hour exam that consists of 120 questions about lubrication fundamentals and grease types, selection, manufacturing, applications, maintenance, testing, etc.

CERTIFICATION EXAM This certification is offered during the NLGI Annual Meeting (once per year).

• •

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The 2021 NLGI Annual Meeting will be held in Tucson, AZ at Loews Ventana Canyon Resort, September 27 – 30, 2021.

Individuals employed by a member company taking the exam will receive a discounted fee. Individuals employed by a non-member company are still encouraged to take the exam; however the fee will be higher. Please view our Annual Meeting registration/pricing information for more details.

Recommended Study Materials

MANTAINING CERTIFICATION • Renews every 3 years • Renewal fee $100 USD • Renewal criteria Certification is an indicator that the individual possesses a high level of expertise in the field of grease. NLGI recognizes CLGS certified individuals as grease industry experts. CLGS certification will serve as a useful tool for employers to screen potential employees and for OEMs and end users to ensure that consultants and suppliers are qualified to make grease related recommendations.

Click Here to See All CLGS Holders.

- 37 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

High-Performance Multiuse (HPM) Grease Column HPM and End-User Promotional Strategy FIRST HPM PRODUCT LAUNCHED! NLGI is pleased to announce the first product approved for the High-Performance Multiuse (HPM) Grease certification!

Castrol’s Tribol GR SW 460-1 is the first product certified against the new NLGI High-Performance Multiuse (HPM) grease specification. In addition, NLGI certifies its enhanced performance in corrosion protection, high load-carrying capacity and low temperature. Tribol GR SW 460-1 is a specialized product for main bearing applications in wind turbines.

In December 2020, NLGI’s launched its High-Performance Multiuse (HPM) Grease certification and sub-categories with enhanced performance in the following areas: • HPM “Core” Spec • HPM Grease with enhanced Water Resistance (HPM + WR) • HPM Grease with enhanced Salt Water Corrosion Resistance (HPM + CR) • HPM Grease with High Load Carrying Capacity (HPM + HL) • HPM Grease with enhanced Low Temp Performance (HPM + LT) NLGI decided to expand its certification program, recognizing that updated specifications may better serve current advanced materials, technologies and applications. In Fall 2019, NLGI

partnered with the Center of Quality Assurance to administer the program and conduct qualification testing. The initial focus of HPM is on premium grease in a variety of bearings and applications which require similar lubricating properties. Future specifications may include high temperature and/or long life.

“We’re thrilled to announce Castrol’s Tribol GR SW 460-1 as NLGI’s first HPM product to market. Congratulations to Castrol for working diligently the past six months on certifying this product. Since NLGI does not dictate chemical, additive, lubricant or viscosity properties, formulators are free to get creative in order to create viable, quality products that meet HPM specifications. Castrol’s Tribol

GR SW 460-1 product has done just that. We are excited to see it in the marketplace!” said Crystal O’Halloran, NLGI Executive Director.

To view Castrol’s press release, click here.

For more information on HPM specifications and how to register your products, click here or contact NLGI HQ at nlgi@nlgi.org.

FREQUENTLY ASKED QUESTIONS I’d like to help spread the word about HPM. Does NLGI have any guidelines around doing so?

Yes. Please click HERE for the marketing guidelines on promoting HPM. Please contact NLGI for a sample HPM logo for internal and external use.

How do I certify my product(s)?

NLGI has partnered with Center of Quality Assurance (CQA) to administer this program. A five-step process is required to register your products. Please visit HERE for information on how to download the application documents.

Where can I find a copy of the HPM specification?

You can find the HPM specification HERE. For more information, please contact NLGI HQ at 816-524-2500 or CQA at 989-496-2399

- 38 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

High-Performance Multiuse Grease

Easy to identify

NLGI

ADVERTISE WITH NLGI

The NLGI Spokesman Magazine is published bi-monthly (6 issues per year) in digital format only.

CIRCULATION INFORMATION The NLGI Spokesman is a trade publication sponsored by the National Lubricating Grease Institute. The circulation reaches over 45 countries worldwide.

CLICK HERE to download The Spokesman rate card.

CLICK HERE to download the nlgi.org website advertsing rate card.

Inquiries and production materials should be sent to Denise Roberts at NLGI (denise@nlgi.org)

2021 NLGI Digital Spokesma

n

ADVERTISING RATES

The NLGI Spokesman Magazine is published bi-monthly (6 issues per year) in digital format only.

2019 Spokesman Advertising

CIRCULATION INFORMAT ION The NLGI Spokesman is a trade publication sponsored by the National Lubricating Grease Institute. The circulation reaches over 45 countries worldwide.

READERSHIP Manufacturers, suppliers, marketers, distributors, technicians, formulators, scientists, engineers and consumers of lubricating greases.

ADVERTISING DEADLINE S January/February ................... Janueary 11 March/April ....................................March 1 May/June ..........................................

May 3 July/August ........................................July 5 September/October ............... September 6 November/December ............. November 1

Ad Size

Rates (includes color) / Display

1 Issue

3 Issues

All 6 Issues

$ 1375

$ 1300

$ 1265

$ 1375

7-1/4” x 9-1/2”

*Back Cover

$ 1300

$ 1265

$ 1375

7-1/4” x 9-1/2”

Full Page

$ 1300

$ 1265

$ 1100

$ 1055

$ 1015

WxH

7-1/4” x 9-1/2” 7-1/4” x 9-1/2”

2/3 vertical

$ 985

1/2 island

$ 950

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$ 865

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4-3/4” x 7-1/2”

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ONLINE/DIGITAL MAGAZINE Live Area: 7-1/4” x 9-1/2” Trim: 8-1/4” x 10-3/4” Bleed: 8-1/2” x 11”

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Images/Files should be at least 200 dpi for best quality (JPEG, TIFF or PDF format)

*Premium positions are on first come, first serve basis; contact Denise Roberts (816.524.2500 / denise@nlgi.org).

• All rates are per insertion, in U.S. Dollars and are based on advertiser supplying complete electronic files in JPEG, TIFF or PDF format.

• All rates are net due to NLGI. Ad agencies and 3rd parties need to add their commissions and fees on top of the net rate.

• NLGI non-members add 40% to rates listed above.

• All advertisers must pay in advance by materials deadline date.

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CONTACT Inquiries and production materials should be to Denise Roberts at NLGI (denise@nlgi.o sent rg)

- 39 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

VERTICAL

SPOKESMAN

NLGI

READERSHIP Manufacturers, suppliers, marketers, distributors, technicians, formulators, scientists, engineers and consumers of lubricating greases.

Check out the NLGI Store Click the sections below to learn more.

nlgi.org/store

NLGI RESEARCH GRANT REPORTS

Grease Lubrication of New Materials for Bearing in EV Motors 2019 - University of California – Merced

Strategies for Optimizing Greases to Mitigate Fretting Wear 2018 - The University of Akron

Determination of Grease Life in Bearings via Entropy 2017 - Louisiana State University

Summary & Full Reports Available

Available to Members Only

Login to the members’ only area to read the report today: https://www.nlgi.org/my-account/

- 40 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

ASTM D-3527 Retrospective NLGI’s new series of High Performance Multiuse (HPM) Grease Specifications has now been introduced with a core specification defined (HPM) along with enhanced performance categories for High Load (HL), Low Temperature (LT), Corrosion Resistance (CR) and Water Resistance (WR). Work has now begun on additional specifications to define specifications around high temperature and long life greases. A steering committee has been formed and has begun discussion around this topic including the development of a new high temperature bearing rig test which will be a critical part of this discussion. Additionally, NLGI and ASTM are working closely together to help improve repeatability of the current high temperature rig test (ASTM D3527) which is still a key part of NLGI’s Automotive Service Greases classification system commonly referred to as GC-LB. With this in mind, NLGI would like to highlight the development work around the ASTM D3527 high temperature test rig as part of the work surrounding the GC-LB specification which was initially introduced in 1989. We offer a reprint of a Spokesman article from 1977 in which D. J. Sargent “reviews the activities associated with the development of ASTM Standard D-3527-76, Standard Test Method for the Life Performance of Automotive Wheel Bearing Greases…under the jurisdiction of ASTM Committee D-2.”

- 41 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

- 45 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021