EUROGREASE. april/may/june

2013 2 april/may/june EUROGREASE grasa greix - koipea schmierfett smeervet plastické maziva smørefett grasso γρασσο grusu mazive masti voitelurasva CMa3Ka mazacie tuky smørefedt gres graisse únsoare smurfeiti smar plasticzny kenozsir smörjfett lubricating grease Review 2013 ELGI AGM ELGI Board New ELGI Members 2014 AGM Dubrovnik Call for Papers Biodegradable Lubricating Greases 20 Years Ago vs. Today 2011 NLGI Grease Production Survey Main Bearing Lubrication for Wind Turbines A Systematic Approach for Grease Selection

Stability in performance, durability of operations, essential ingredients for achieving busines goals. ANDEROL has the proven expertise to face challenges, resulting in increased and consistent plant efficiency, reduced labour and material costs, providing you with flexible and customized solutions for all your lubrication needs. Offering full reliability with our extensive range of H1 food grade lubricants, our specialization in gas compression and vacuum applications, serving industries all around the world. A constant aim for improvements and solutions is the core of our business. Rise to the occasion with us! ANDEROL BV P.O. Box 1489 6201 BL MAASTRICHT +31 (0)43 352 41 90 +31 (0)43 352 41 99 info@anderol-europe.nl www.anderol-europe.com

Chairman: Terry Dicken Global Lubricants Ltd. Sandwell Bus.Dev. Centre Oldbury Road Smethwick West Midlands B66 1NN United Kingdom (T): +44 121 544 3638 (F): +44 121 544 6505 (M): +44 7710 754 382 terry@globallubricants.co.uk Vice-Chair: Leandro Muntada Brugarolas S.A. Camino de la Riera 36-44 P.I. Cova Solera; 08191 Rubi Barcelona, Spain (T): +34 93 588 3100 (F): +34 93 697 6313 lmuntada@brugarolas.com Secretary: Josef Barreto-Pohlen Tunap Industrie Chemie GmbH & Co Bürgermeister Seidl Strasse 2 D-82515 Wolfratshausen, Germany (T): +49 8171 1600 75 (F): +49 8171 1600 69 (M):+ 49 151 150 59 421 josef.barreto@tunap.com Treasurer: Peter-Paul Mittertreiner Lubricant Consultant Hemonylaan 26 1074 BJ Amsterdam; The Netherlands (T): +31 88 231 1820 (M): +31 (0) 6317 56098 pp.mittertreiner@prorail.nl Director /Editor: Valentina Serra-Holm Nynas AB P O Box 10700 SE-121 29 Stockholm, Sweden (T): +46-8-602 12 94 (F): +46-8-81 62 02 (M): +46-70-284 89 40 valentina.serra-holm@nynas.com Director: Eddy Stempfel Fuchs-Lubritech GmbH Werner-Heisenberg-Strasse 1 D-67661 Kaiserslautern, Germany (T): +41 34 445 3375 (F): +49 6301 3206 940 eduard.stempfel@fuchs-lubritech.de Director: Rolf Quermann Carl Bechem GmbH Weststrasse 120 D-58089 Hagen, Germany (T): +49 2331 935 1122 (F): +49 2331 935 1129 quermann@bechem.de april/may/june 2 Content Podium (T.Dicken) 2-3 ELGI Board 3 Thank you note (L. Flabbi) 4 New ELGI Members 4 2014 AGM Call for Papers 5 Biodegradable Lubricating Greases 20 Years Ago vs. Today (E.M. Stempfel) 6-17 2013 AGM Photos 18-21 2011 NLGI Grease Production Survey (C. Coe) 22-26 Main Bearing Lubrication for Wind Turbines A Systematic Approach for Grease Selection (D.A. Pierman) 28-38 Forthcoming events 40 Eurogrease subscription & advertising rates www.elgi.org / publications Cover photo: Director: Andreas Dodos Eldon's SA 20 Souliou Street 14343 Athens, Greece (T): +30 210 5596 441 (F): +30 210 5596 444 (M): +30 6974600922 andreas.dodos@eldons.gr Office Manager: Carol Koopman ELGI Hemonylaan 26 1074 BJ Amsterdam; The Netherlands (T): + 31 (0) 20 6716 162 (F): + 31 (0) 20 6732 760 (M): + 31(0) 62322 6180 carol@elgi.demon.nl carolkoopman@hotmail.com www.elgi.org 3 Treasurers past & present: Gerhard Schmidt, PP Mittertreiner, Tim Hutchings 25 th ELGI AGM Amsterdam The opinions expressed in this magazine are not necessarily those of the ELGI Board and/or the publisher. No responsibility is accepted for the accuracy of the information contained in the text or illustrations. EUROGREASE 2 april/may/june 2013 1

Terry Dicken ELGI Chairman It is with great pleasure to write this podium letter following our 25 th AGM held in Amsterdam, the city which is home to the ELGI, and for this key event I am happy to report our highest number of attendees ever with over 350 delegates registered from 31 different countries. It was also nice to welcome back three of our retired board members Luciano Flabbi, Gerhard Schmidt and Tim Hutchings. Luciano & Gerhard have now also retired from the industry but are in good health and a pleasure for both to participate at an AGM they have not attended for several years. And who better than Graham Gow could open our conference with a reflection on how ELGI was born and the difficulties experienced in the first few years of our existence. Today, ELGI is a vibrant organisation with a membership of 150 members from a worldwide base, is in a good financial state and has 5 working groups actively addressing the issues relating to our industry and an annual general meeting swelling in numbers not only from delegates but from exhibitors, sponsors and presenters. To mark this milestone event your board agreed to spend more on its organisation than usual resulting in a fine venue to accommodate delegates and present our papers. Excellent facilities enabled our exhibitors to have a high footfall and a lot of interest in their products and services while also providing space and time for constructive business discussions. The whole programme of events accumulated in a spectacular gala dinner held at the restored Maritime Museum on the harbour IJ with our delegates arriving from the hotel on a flotilla of boats, having a chance to enjoy an aperitif on a spring evening while slowly passing through the canals of Amsterdam. Many thanks to our excellent band who provided a night of varied music keeping many of our members on the dance floor most of the night. This year s AGM also saw the election of two new board members including the election of our first lady to join the ELGI board, Valentina Serra-Holm who brings with her a wealth of experience not only from an engineering viewpoint but on the worldwide base oils market. Andreas Dodos was also welcomed to the board. His experience in grease manufacture combined with his work as Chairman of ERGTC will be a valuable asset to our activities; we look forward to their contribution and input. It was also a pleasure that Eddy Stempfel was re-elected and will continue his technical contributions to the board for a further 3 years. At the same time however, it was sad to announce that Jean Hirigoyen stepped down from the board after 15years. Jean was a very valuable member of the board with his considerable commercial abilities and knowledge of the industry playing an important part in the organisation of our AGM's, not to mention his superior knowledge of fine wines! He will be greatly missed but will continue to assist the board in other roles in the future. In addition it was a pleasure to present Jaime Spagnoli the Best Paper Award for his paper on False brinelling test (Riffel) for wind turbine grease which he presented last year at our conference in Munich; and I would like to take this opportunity to remind you that if you would like to present a paper at next year s conference, where the theme next year will be "High Temperature Extreme Conditions", please submit an abstract to the ELGI office by the end of October. If you would like to view the full programme of this year s events and delegates list, you can do so by downloading our ELGI App; scan the link herewith with a QR Reader. Details of the 2013 AGM will 2 EUROGREASE 2 april/may/june 2013

remain on the App for a further month or so before being replaced with details of next year s AGM. This will be held at the Radisson Blu Hotel just a few kilometres from the wonderful UNESCO World Heritage city of Dubrovnik, Croatia during April 26 th -29 th 2014 (www.radissonblu.com/resort-dubrovnik). We look forward to welcoming as many of you as possible to attend this event and if you re interested in presenting a paper, exhibiting or want to take advantage of our many sponsorship opportunities please contact the ELGI office. So on behalf of the board I would like to thank all the presenters, exhibitors, sponsors and of course the delegates who made our 25 th Anniversary AGM such a wonderful event but most of all we would like to offer our warmest thanks to all the members who have made the past 25 years so successful for us. Jean Hirigoyen receiving a farewell gift from Terry Dicken Jean Hirigoyen & Terry Dicken New board members Andreas Dodos & Valentina Serra-Holm welcomed by Terry Dicken ELGI Board 21 st April 2013 (Top row) Josef Barreto-Pohlen, Terry Dicken (Middle row) Eddy Stempfel, Rolf Quermann (Bottom Row) Jean Hirigoyen, Carol Koopman, Peter-Paul Mittertreiner EUROGREASE 2 april/may/june 2013 3

Lucia & Luciano Flabbi Just a short note of thanks from Luciano Flabbi, former board member 1992-1998 I left the ELGI Board at the end of the last century after six year of service, during that time I was mainly involved in the many technical aspects of the organisation. Of course I was very pleased to attend this AGM in 2013, as I am presently retired, it was a way to once again be in contact with my former job and experience how the Institute operates. Compared to my times, the number of attendees at the AGM has dramatically increased, it has more than doubled, and in addition I noticed that the "globalisation" of the industry has attracted a number of countries that were missing in the past. It was good to see so many new Working Groups are active and well attended alongside the well established Test Methods Working Group and the fact that there is a good working relationship with our colleagues at the NLGI. I think that Amsterdam was the best location to celebrate the 25 th Anniversary because it is the place where everything began and where the ELGI has its headquarters. In addition Amsterdam is a town of great appeal and played a key role in the history of Europe and in the development of the Western culture. The organization of the event was very professional, including the host hotel, location of the gala dinner and the entertainment: the trio players during the welcome party, the folk dancers introducing the General Meeting and the band playing at the gala dinner. I wish the ELGI another successful 25 years!! And thank you for inviting me back. New ELGI Member Mr. Benoît Decottignies SOGELUB S.A. (Producer) BE 7522 Marquain, Belgium Tel : +32 69 59 09 49 Fax : +32 69 21 44 74 benoit.decottignies@sogelub.com www.sogelub.com www.sogelubglass.com 4 EUROGREASE 2 april/may/june 2013

Call for 2014 Technical Papers "High Temperature Extreme Conditions 26 th ELGI AGM 26 th 29 th April 2014 Radisson Blu Hotel Dubrovnik Croatia Papers that tie in with the 2014 theme "High Temperature Extreme Conditions : Consider greases designed for excellent performance under high temperature conditions e. g. in steel plants or cars, will be given high priority Machine parts lubricated with grease drafted for high temperatures and grease components like base oils and additives that enhance high temperature stability of greases will also be given priority. Other topics of interest to the grease industry are welcome and will be considered too. The cut off date for submitting your paper proposal is 31 st October 2013 (T) +31 20 67 16 162 carol@elgi.demon.nl www.elgi.org EUROGREASE 2 april/may/june 2013 5

Biodegradable Lubricating Greases 20 Years Ago vs. Today Presented at the 25 th ELGI Annual General Meeting 2013 Amsterdam The Netherlands Eddy Stempfel Fuchs Lubritech GmbH Kaiserslautern - Germany eduard.stempfel@fuchs-lubritech.de Eddy Stempfel worked in the Lubricants Industry (ASEOL AG, Shell Aseol AG and Fuchs Lubritech GmbH) for the last 43 years. He had several jobs during these years e.g. R&D greases, synthetic fluids and industrial lubricants. In the mid seventies he was assistant to the LOBP and grease plant manager. He became Head of the R&D and Analytical Laboratory. In 1985 he became manager of the department R&D and Analytics, which included the local technical support. He was a member of the company management and management representative for Q-HSE. In 2005 he joined Shell Global Solutions as a Product Application Specialist for Food Grade & Biodegradable Lubricants and took over the global product manager role for the food grade lubricants. Eddy joined Fuchs Lubritech GmbH, Division Food 1 st October 2010 as Global Product Manager and Application Specialist. Eddy s background is chemical engineer. He lectures at several associations and he published several papers on biodegradable and food grade lubricants (two of which he received an award for). Eddy Stempfel is member of Fuchs-Lubritech Global Food Sector Team and ELGI (European Lubricating Grease Institute), Board Director. E.M. Stempfel, Fuchs Lubritech GmbH Foreword We now celebrate the 25 th anniversary of our institute. During one of our board meetings last year we decided it could be a nice and interesting add-on to the AGM 2013 program to re-iterate an almost 25 year old paper, which has been presented at both NLGI and ELGI AGM s in the early nineties and to have a look on what happened in the meantime to the Biodegradable Grease Technology. The original paper Biodegradable Lubricating Greases Developments, Applications, Trends was developed by and presented by E.M. Stempfel and L. A. Schmid of ASEOL AG, Bern, Switzerland. The initial paper has been awarded by Chevron U.S.A. with the Chevron U.S.A. Award for the best marketing paper presented during the 57 th AGM of NLGI in October 1990 in Denver, CO. 1. Introduction Our environment is the basis of all that lives on Earth. But this very environment is being stressed to an ever-increasing extent by the emissions and pollutions caused by us. It is therefore hardly surprising that great efforts have been made in recent years to develop and employ more and more products and technologies that are compatible with the environment. In Europe this evolution has already found its way into the lubricants field. This is very easy to understand when one thinks of the quantities of lubricants that find their way into the environment direct as a result of loss lubrication. The paper describes the experience acquired to date and future possibilities for the development and application of biodegradable lubricating greases on the European market. 6 EUROGREASE 2 april/may/june 2013

Biodegradable lubricants, having a minimum impact on the environment or giving no cause for complaint, whatever these terms may mean, have attracted increasing attention in Europe in the past few years. This has not occurred simply by chance, when one thinks of the vast quantities of lubricants that find their way virtually direct into the environment as a result of loss lubrication. On the Swiss market alone they amount to about 4000 tons. To this must be added the unknown figures due to leakage and breakdowns, e.g. in tunnels, on construction machinery, dredgers and the like, where lubricants are lost. Not the least for this reason has the political pressure increased, Le, both manufacturers and users are being called upon, to search for alternatives to these materials, which are more neutral with respect to the environment. lt may be taken for granted that, in the future, legal directives will be issued for certain fields of application, which stipulate that such new types of lubricant shall be used. This trend has already commenced with liquid lubricants. It began with the introduction of biodegradable oils for outboard engines towards the end of the 70s and then made marked advances in the early 80s in the area of oils for chain-saws. Fig. 1 shows the present applications that are possible for biodegradable liquid lubricants on the European market. Biodegradable greases have only come into the foreground in the last two years. The authors envisage uses for this new generation of lubricating greases in agriculture, the central lubrication of truck chassis, in waste water purification plants, hydro-electric power plants and for the lubrication of rails, wheel flanges and switches on the railways. That the history of tribology in its widest sense goes back thousands of years can be seen in Fig. 2. Even in those days lubricants found their way direct into the environment; of course the quantities were much smaller than they are nowadays. However, the lubricants employed exhibit close similarity to the biodegradable lubricants used today. It is therefore not astonishing that the formulating chemists have turned their attention to these old ideas. The number of raw materials, which has risen enormously since then, naturally offers more opportunities now to select suitable ones. 1.1 2013 Update In fact no major and significant changes happened during the last two decades. Surely new applications have been found and developed, testing and definitions (e.g. eco-labels) have been fine-tuned, developed further and finally the overall sold volumes have increased. However this increase in sales was mainly based on the fact that more and more countries and users have recognized the potential for such products and not because legislators would have changed their support for such lubricants. A still very often seen hurdle in end-user minds is that biodegradable lubricants are still more expensive than standard lubricants and, if there is no pressure from legislators, they therefore do not use them. The public understanding changed as well. 20 years ago biodegradability was the almost single argument and became a sort of hype. Today manufacturers and end-users look at much more diversified and specific requirements such as ecotoxicity, renewability and OEM approvals in combination with energy saving potential and biodegradability. 2 Biodegradability Terms like compatible with the environment, nontoxic, ecologically unquestionable are expressly forbidden according to Swiss Law (Materials Decree, Poisons Law). And this is not without justification because the user could mistakenly believe that such products can be emitted to the environment without question, even that they might be useful to the environment. But when leaks or accidents occur, the same measures have to be adopted as for lubricants based on mineral oils. In many parts of Europe waste biodegradable lubricants have to be disposed of as special refuse. But this does not mean that such new lubricants are consequently unnecessary. By using them for specific purposes the strain on the environment can certainly be lessened in the long run. The idea that the authors would like to pass on at this juncture is that, in comparison to substances based on mineral oil, such products "impose less strain on the environment". Moreover, when saying they are "biodegradable', the relevant test method and the values measured should always be quoted. The most important method used in the branch today, unfortunately almost the only one available for testing products that cannot be mixed with water is the test according to CEC-L-33-T- 82.This test method was originally developed by the Swiss Federal Establishment for Testing Materials to determine the biodegradability of oils used in two stroke outboard engines. The CEC method is used in aqueous surroundings with bacteria cultures from sewage works. The biodegradability of a lubricant is plotted over a EUROGREASE 2 april/may/june 2013 7

period of 21 days in comparison to white oil and diiso-tridecyladipate. The results are evaluated by measuring the degradation of the CH-QT-bands at 2930 cm -1 with an infrared spectrophotometer. In this test white oil attains a degradability of 20-30%, di-iso-tridecyladipate a value of almost 100%. No further reference will be made here to details of the method. Adequate information can be found in the relevant literature. The set-up used for the CEC test is illustrated schematically in Fig. 3. Unfortunately, there is as yet no official method which takes all important environmental criteria into account (water, soil, air and light). Here there is work to be done, because only a method that is capable of doing this will be able to provide more exact figures on how much better the degradability of such a lubricant is in comparison to mineral oil. 2.1 2013 Update As already mentioned, testing has changed significantly. There were many discussions about the accuracy of the initial CEC-L-33-T-82 method which became later on active status and is now called CEC-L-33-A-93. Some investigation has been done in this method and finally a new method appeared which is called CEC-L-103-12. However all of these methods basically only provide an indication about the primary degradation. New test methods have arisen, well known today as OECD 301x - methods. This set of methods allows a much better assessment of everything, which today is called biodegradable, environmental harmless or friendly. By the way, the statement of the authors of the original paper that nothing is environmentally friendly but may impose less strain on the environment is basically still valid and I can only re-iterate it. It was probably more or less taken as a philosophic statement 20 years ago. Unfortunately in this special case time didn t change the behavior of marketers and we can still find a lot of data sheets, flyers and brochures stating that the indicated product is environmentally friendly or harmless. May be the forthcoming 20 years will change it and this misleading argument will disappear. Some first steps have already been done (e.g.by the technical report CEN/TR 16627 or ISO 14021:1999) requirements are still heavily discussed, these labels are pretty helpful for the end-user and have as well found their way into specific requirements for lubricants used in sensitive areas. 3 Biodegradable greases, components Fundamentally the structure of biodegradable greases is the same as those based on mineral oil. But when choosing the components the biodegradability is the most prominent factor. An overview can be seen in Fig. 4. 3.1 2013 Update Biodegradability according to OECD is still one of the main factors. The requirements have evolved into a scheme where biodegradability of formulation components is even more important than the biodegradability of the overall finished product. Today equal importance is set to ecotoxicology, renewability, technical performance, CO2 balance of raw materials, in fact to the whole life-cycle of the product and its components. 3.2 Base fluids Fig. 5 shows the possibilities remaining for the choice of suitable base fluids. They can be divided into two main groups: a) Base oils miscible with water b) Base oils non-miscible with water The base oils that can be mixed with water are almost exclusively glycols. Most frequently used today are monopropylene glycol and polyethylene glycols with an average molecular weight of 200 to 1500. The biodegradability decreases notably with increasing molecular weight. On account of their poorer biodegradability, polypropylene glycols are used less in this sector. Ethylene oxide/propylene oxide mixed polymers can be appreciably varied as regards their viscosity, biodegradability and solubility in water and have therefore also found applications in this field. The advantages of this family of base fluids, such as resistance to ageing and hydrolysis, are offset against the drawback of solubility in water and incompatibility with mineral oil. In addition, the very different behavior relative to sealing materials has also to be taken into account. The base oils that do not mix with water, which are mainly used in this new generation of lubricating greases, can also be divided into two groups: a) Native oils (mainly vegetable oils) b) Synthetic esters As already mentioned the development of special labels for this lubricant family (e.g. Blue Angel, Nordic Swan, EU Ecolabel) took place during this time as well. Although some of the respective 8 EUROGREASE 2 april/may/june 2013 Chemically, native oils and synthetic esters exhibit basically the same structure. Consequently their properties are also very similar. As regards resistance to ageing and their behavior at low

temperatures, synthetic esters offer distinct advantages over vegetable oils. But these advantages are only acquired by paying a notably higher price. Both of the groups described are relatively prone to hydrolysis due to their chemical structure. Beside this, the vegetable oils exhibit lack of saturation in their molecular structure (double bonds), which can be very neatly expressed by their iodine value. An overview of the iodine value of the main vegetable oils can be seen in Fig. 6. The magnitude of the iodine value is directly related to the resistance to ageing of vegetable oils. Here the synthetic esters offer more opportunities. Nowadays esters are available in an extremely wide range of varieties. For instance the iodine value of esters can be reduced to zero and the molecule sterically hindered, so that notably better ageing properties and resistance to hydrolysis can be attained. However, these improved properties are to be paid by a much higher price. Therefore when formulating lubricating greases, it is necessary to consider what properties are needed and what base oils meet this requirement profile. The vegetable oils mostly used nowadays are rapeseed and castor oil. Among the esters it is mainly trimethylolpropane-, pentaerythrite- or neopentylpolyolesters of a number of fatty acids. An advantage of these two groups of base oils is that they mix readily with mineral oil, thus resulting in a satisfactory compatibility with "normal' lubricating greases containing the same kind of thickener. A summary of the biodegradability of different base fluids and their respective chemical and physical properties is given in Fig. 7 and 8. 3.2.1 2013 Update Regarding base fluids there is a much bigger variety of different types available today, especially in the range of synthetic esters (saturated, unsaturated) and specially treated vegetable oils. A big step forward is the fact that today formulation chemists can usually get complete data sets of raw materials consisting of biodegradability, renewability, toxicity 3.3 Thickeners The well-known kinds of thickener can all be used, bearing in mind, though, that inorganic thickeners such as clay or silica are not biodegradable. The authors regard the use of the following thickeners to be appropriate: Lithium-12-OH stearate Calcium- 12-OH stearate Lithium/calcium soaps Aluminum complexes Here, too, the choice of the thickener is again greatly influenced by the requirement the grease has to fulfill. 3.3.1 2013 Update There was no significant change regarding the thickeners in use. The ones mentioned above are still pre-dominant. Today one might add to the list Calcium complex and Lithium complex technology as well but may skip the Aluminum complexes. A big step forward in this case is the introduction of the so called LuSC-list (Lubricants Substance Classification list). This is a non-limitative list of single substances but of branded additives as well. A really helpful tool! 3.4 Additives Up to the present very few additives have been offered specially for use with biodegradable products (tackiness agents, thickeners for oils and pour point depressants). Consequently the formulating chemist has to resort to those additives that are available on the market. Wherever possible, pure additives free from mineral oil and heavy metals should be used. The additive-response of vegetable oils and synthetic esters may be regarded as very good. With glycols, though, the scope is very much less. Common additives are: Antioxidants: amines and phenols (BHT) Anti-corrosion: fatty acid derivatives amines EP/Antiwear: S P compounds, Dithiocarbamates (ashless) 3.4.1 2013 Update Regarding additives we can recognize a big step forward. Additive suppliers have investigated in new technologies and included the ecotoxicological requirements which are part of the set-up of different standards and in the different ecolabels. Today one can chose from a big variety of additives which fulfill all relevant environmentally related requirements (e.g. LuSC-list). 3.5 Manufacturing When manufacturing biodegradable lubricating greases close attention must be paid to the chemistry of the base fluids. The manufacture in autoclaves or contactors does not strike the authors as being appropriate because the loads on the base oils (especially vegetable oils and synthetic esters) by the pressure exerted and the water of reaction that is present at the same time EUROGREASE 2 april/may/june 2013 9

are too high, so that the base oils are saponified at the same time. This leads to a reaction that is difficult to control and correspondingly varying end products. Such greases have a marked tendency to saponify later, manifested by poor keeping properties (hardening). Production with pre-made soaps in an open kettle has a less harmful effect and is therefore preferable. Since pre-made thickeners can prove to be a cost factor that may not be underestimated the authors have devised a process which permits "in situ" saponification of vegetable oils in an open kettle, using suitable protective chemicals. 3.5.1 2013 Update Manufacturing of greases basically didn t change over the last two decades. Therefore they are usually manufactured by the same procedures as 20 year ago. There was one new idea/technology, which became of some interest: Producing greases via Microwave. This interesting new method has been developed by University of Northern Iowa researchers and an Iowa-based industrial microwave company. More information about this technology can be gathered from several papers presented by L. Honary during recent NLGI and ELGI AGM s. 4 Properties of biodegradable lubricating greases Apart from considering the price, the user will ask where he can render a contribution to conservation of the resources and the environment by using biodegradable greases. To answer this he must have a clear opinion of the different characteristics of these greases compared to grease based on mineral oil, Fig. 9 gives an overview of the main properties of biodegradable lubricating greases. For comparison the authors chose ordinary commercial grease based on mineral oil. All the biodegradable greases illustrated achieve a degradability of more than 80% in the CEC-L-33-T-82 test. The greases illustrated are built up of the following: Thickeners A Li/Ca- 12-OH stearate B Li/Ca- 12-OH stearate C Li/Ca-12-OH stearate D Li/Ca stearate Base fluids A Mineral oil (paraffinic) (150 mm 2 /s at 40 C) B Synthetic ester (88 mm 2 /s at 40 C) C Native oil /synth. ester 1:1 (85 mm 2 /s at 40 C) D Native oils (80 mm 2 /s at 40 C). Additives A Antioxidant/corrosion/antiwear/EP/tackiness (not ashless) B same as A but ashless C same as A but ashless D Antioxidant/corrosion/tackiness (ashless). 4.1 Static resistance to oxidation The values shown in Fig. 9 for the static oxidation test correlate very well with the content of vegetable oil, which was used as base fluid. The tests were performed with pure oxygen at 100 C in the oxidation bomb (ASTM-D-942). These relatively poor properties cannot be brought to a level comparable with the product based on mineral oil even with additives. For the applications considered the authors do not see any absolute necessity (loss lubrication). The limited storability resulting from the poorer resistance to ageing of such greases has to be taken into account by the manufacturer and the user. One European manufacturer therefore recommends on his cans that a grease base on rape-seed oil should be used within one year. 4.2 Working temperature range Because of their chemical structure, vegetable oils are notably less resistant to ageing, thermal stresses and hydrolysis than mineral oils. This restricts the applications of the greases made from them. The upper limit for the working temperature is around 90 C. At higher temperatures thermal degradation soon becomes apparent. The working temperature range, however, can be extended by adding synthetic esters. The authors are of the opinion that with 50% of a selected synthetic ester and corresponding additive(s) the working temperature ranges of a normal" lithiumsoap EP grease can easily be attained. If a mixture of fully synthetic base oils is used, the properties at both low and high temperatures can be definitely improved. But a considerably higher price has to be paid as a result. 4.3 Low-temperature properties Vegetable oils consist of a wide range of fatty acid esters. That is why their low-temperature properties can by no means be compared with those of mineral oils. For the latter the pour point is utilized as the main characteristic value for the comparison. For vegetable oils this value yields very little information with regard to the lowest working temperature. Owing to their chemical 10 EUROGREASE 2 april/may/june 2013

structure as described, vegetable oils tend to crystallize into long-chained esters of fatty acids well above the measured pour point. For rapeseed oil, for example, a pour point of -20 C is measured, but if this oil is stored at -15 C for one week it will no longer flow. This special behavior can be documented very well by long-term low-temperature penetration measurements. It can be influenced only to a limited extent down to -30 C by additives and has to be allowed for when selecting the base oil for a given application. Fig. 10 shows the results of such measurements, for example, on greases based on rape-seed oil, rapeseed/ester and paraffinic mineral oil. The measurements were performed at NLGI 2 grade greases. It should be noted that the viscosity of the base oil used for the tested greases differed somewhat. 4.4 Antiwear/EP properties By using commercial additives biodegradable greases can be given similar properties to those based on mineral oil. The pronounced polarity of the vegetable oils and synthetic esters can lead to competitive reactions on metal surfaces, though. To obtain the same properties as mineral oil based greases it is therefore necessary in most cases to add a higher proportion of additive. Unless a typical EP grease has to be formulated (e.g. TIMKEN> 40 lbs.) the very good natural lubricating properties of vegetable oils are often quite sufficient to assure protection against wear. 4.5 Prevention of corrosion Here the same applies as to antiwear/ep properties. Their excellent affinity on metal surfaces provides vegetable oils certain natural anti-corrosion properties. In many cases there is no need for any additives, but if they are used the possibility of competitive reactions must be taken into account. To obtain the same properties as mineral oils it is sufficient in most cases to add only small quantities of appropriate additives. 4.6 Dynamic resistance to oxidation As screening test the authors used a method developed in their own company Fig. 11. The four bearings tested were axial deep-grooved ball bearings type FAG 51209 with an outside diameter of 70 mm. The bearing cage was open on one side and was filled with 5 g of grease. The bearing ran at a speed of 400 min -1 and was loaded with 9.5 kg. The test temperature is open to choice and can reach 200 C. Also the duration of the test is optional. The following points can be evaluated: a. throw-off tendency b. hardening of the grease through the startup torque - formation of oil carbon and changing the aspect. Aspect-evaluation is performed visually. A small amount of the grease is removed from the bearing daily and applied to a glass plate. Every time grease is removed, an equal amount is added as lubricant. The tests are performed in comparison to known greases that have been proved in practice. Fig. 12 shows the results obtained with greases A to D at 140 C and 110 C. With this test method the marked dependence of the ageing on the composition of the base oil is evident. Lubricating greases A (mineral oil) and B (fully synthetic) exhibit virtually the same lifetime. Their lubricating property is retained over long periods of time, both at 110 C and 140 C. At the higher temperature grease B actually yields better results. With greases C (vegetable oil/synthetic ester 1:1) and D (vegetable oil) the performance decreases with increasing content of vegetable oil. Thus grease D just attains 190h at 140 C and 400h at 110 C, before lubrication of the bearings ceases to be effective. 4.7 2013 Update It s not the intention of the author to comment on all above paragraphs about properties and performance of biodegradable greases. This was the topic of many other papers written and presented during the last two decades. However and as a general comment one can recognize that both technology in manufacturing and development in formulations have seen big steps forward. The actual variety in available raw materials makes it much easier, to formulate high performing biodegradable lubricating greases today. 5 Applications, trends Vegetable oil based lubricating greases can be used at temperatures between -20 C and +90 C. Even without special additives they exhibit good properties as regards lubrication capacity and protection against corrosion. The authors can therefore envisage this new generation of greases being used in all situations where purely loss lubrication at short intervals is involved. With partly and/or fully synthetic greases some of the limits imposed by vegetable oils can be appreciably extended. However, before these greases are used, their price/performance ratio must be carefully examined. The authors envisage EUROGREASE 2 april/may/june 2013 11

realistic scope for applications of biodegradable greases in the following fields. Centralised lubricating systems an trucks and in industry Chassis lubrication on trucks Construction and excavating machines employed in aquatic nature reserves Railroad wheel flanges, tracks and switches Waste water purification plants Open gears Agricultural machinery Machinery for foodstuffs Various practical examples are illustrated in Fig. 13 to 24. Especially for the central lubrication of chassis, railway switches and agriculture machines the greases described have already secured a share of the market in Europe. More widespread application largely depends on our preparedness to take environmental protection seriously and to accept the higher costs that it involves. 5.1 2013 Update The list provided in paragraph 5 regarding lubricating greases is basically still valid as well as the comments. Today one could add as well the Offshore Wind Power sector. One might set some question mark regarding the machinery for foodstuffs and in agricultural machinery. There is some competition in this case with using food grade lubricants instead. A combination of both biodegradability and food grade is technical possible and such lubricants are already available. This could be an alternative in lubrication of agricultural machinery but certainly not in general for all common food machinery. One reason might be the biodegradability, which implies the presence of humidity and bacteria. Especially the latter one is not as preferable when it comes to hygiene in food processing environment. 6 Conclusions For novel, biodegradable lubricants the future offers a great potential. Oils used for chain-saws and hydraulic systems are already quite widespread in Europe. For greases this evolution is only just starting. But almost daily new scope for the application of biodegradable lubrication greases is found. The suppliers of raw materials have also recognized this opening in the market and have lately begun to offer improved base materials for this purpose. Combined with the products offered by the additives industry, the task of the formulating chemists of finding optimal solutions in the future will be simplified. For all applications the results obtained in practice during the coming years will point the way to the breakthrough for these lubricants, because comparison with laboratory tests does not always provide sufficiently reliable information. But the authors would like to warn against using biodegradable lubricants in every region at all costs. Certain applications of these products are clearly limited by the chemistry of vegetable oils and synthetic esters, and this cannot be invented anew. With this paper the authors aimed at providing a brief outline of the opportunities open to lubricant manufacturers, especially as regards lubricating greases. The authors are convinced that the approach adopted is right and should be pursued further with all the energy available. This would also enable the often decried mineral oil industry to show that it is willing to render its contribution to the environment for the benefit of future generations. It is extremely important though, in this field, to know and accept that only close collaboration between machinery manufacturers, lubricant manufacturers, additive suppliers and users can achieve the desired objective. 6.1 2013 Update Most of the above statements are still valid. There was a clear evolvement during the last 20 years regarding this family of lubricants, where the fluids still play a pre-dominant role. Standardization has made a significant step with new standards and eco-marks. Public has become much more aware of the existence of such products and even some legislators made their first mind change (although mainly locally). Nevertheless price performance ratio must be OK. Otherwise the end-user will not go this route. Regarding the global marketplace the European Union Members seem to be still most advanced although for example the United States has made its progress as well. Biodegradability as single argument has mainly disappeared. Much more important today is clearly a much wider view on such lubricants, which includes: Biodegradability Ecotoxicity Life-Cycle Analysis Renewability CO2 Balance Potential Energy Saving Technical Performance 12 EUROGREASE 2 april/may/june 2013

Finally there is still space for improvement to standardize, develop and promote Eco-Lubricants, to do something for our current and future environment, even if it may be slightly more expensive. It is a fact that over the last two decades Eco- Lubricants became a permanent and fully accepted member of the overall lubricants family. Let s see where we stay in 20 years from now. Figure 2: History of Tribology Literature (initial paper) 1 Ullmanns Enzyklopädie der technischen Chemie, Band 11 "Fette + Ole, Verlag Chemie, Weinheim 2 Hubmann, A.; Rapsöl - ein alternatives Basisöl für Schmierstoffe; Mineralöltechnik, 9 (1989) 3 Coordinating European Council for Development of Performance Tests for Lubricants and Engine Fuels. Tentative Test Method CEC-L-33-T-82, 1982. 4 Nagdi K.; Dichtungswerkstoffe für Umweltfreundliche Flüssigkeiten; Ölhydraulik + Pneumatik, 34 (1990), 42-50 5 Stempfel E.M.; Alternative Ausgangsmaterialien für Schmierstoffe; 6. Informationsseminar Biogene Kraft- und Schmierstoffe; Tu Wien, 1611.1989 6 Holde; Kohlenwasserstofföle und Fette, Verlag Julius Springer, Berlin 7 Schaedler; Fette und Öle der Fossilien, Verlag Baumgärtner, Leipzig Literature (2013 Update) 1. Völtz, M.; New CEC test method L-103 for Lubricant Biodegradability. 2. CEN Technical Report 16227:2011 3. Luther R.; EU Ecolabel, CEN Aktivitäten, Nachhaltigkeit: Gibt e seine EU-Strategie für Bio- Schmierstoffe? VSI Seminar, June 2012. 4. USDA 7 CFR Part 2904. Voluntary Labeling Program for Biobased Products. 5. EU LuSC list, 04.03.2013 Figure 3: CEC-L-33-T-82 Test method (schematic) Figure 4: Main components for biodegradable greases Figure 1: Application examples for biodegradable lubricants EUROGREASE 2 april/may/june 2013 13

Figure 5: Base fluids for biodegradable greases Figure 6: Vegetable oils, properties Figure 7: Biodegradability of different base fluids (CEC-L-33-T-82, 21 Days) Figure 8: Comparison of chemical and physical properties of biodegradable base fluids (average values) MINERAL OIL GLYCOL VEGETABLE OIL SYNTH. ESTER Density at 20 C 880 1100 940 930 Viscosity Index 100 100 to 200 100 to 250 120 to 220 Shear Stability good good good good Pour Point -15-40 to +20-20 to +10-60 to -20 Cold flow properties good very good poor very good Miscibility with ---- not miscible good good Mineral Oil Solubility in Water not soluble very good to not not soluble not soluble soluble Seal Swelling slight swelling special materials are indifferent moderate swelling properties recommended Behavior against good poor good good to poor paintings/ coatings Biodegradability 10 to 35 10 to 100 70 to 100 10 to 100 (CEC) % Oxidation Stability good good fair good Hydrolytic Stability good ---- poor fair Sludge Forming good ---- poor fair Tendency Costs 1 2 to 4 2 to 3 4 to 20 14 EUROGREASE 2 april/may/june 2013

Figure 9: Biodegradable greases, properties comparison with mineral oil based grease Grease Designation Standard A B C D NLGI CLASS NLGI 2 2 2 2 WORKED PENETRATION AT mm/10 ISO 2137 280 280 280 280 25 C BASE OIL COMPOSITION MINERAL OIL PARAFFINIC SYNTHETIC ESTER CASTOR OIL/ SYNTH. ESTER 1:1 BASE OIL VISCOSITY AT mm2/s ISO 3104 150 88 85 80 40 C DROPPING POINT C ISO 2176 190 193 170 180 THICKENER LI-/CA- 12-OH-STEARATE IN SITU MANUF. CONTACTOR LI-/CA- 12-OH-STEARATE PREMADE SOAPS LI-/CA- 12-OH-STEARATE IN SITU MANUF. OPEN KETTLE CORROSION TEST (Emcor) WITH DISTILLED WATER COPPER CORROSION (24H/100 C) FOUR BALL TEST, WELD LOAD OPEN KETTLE Rating DIN 51802 0 / 0 0 / 0 0 / 0 0 / 0 Rating DIN 51811 1 1 1 1 N DIN 51350/4 >2400 2400 2400 1600 TIMKEN OK-LOAD N (lbs) ASTM D 2509 >200 (>45) 160 (35) 160 (35) 68 (15) OXIDATION STABILITY kpa DIN 51808-15 - 25-150 - 400 (100 C/100H) WATER STABILITY, STATIC Rating DIN 51807/1 0 1 1 1 (3H/90 C) ADDITIVES ANTIOXIDANT ANTICORROSION ANTIWEAR/EP TACKINESS (ASH CONT.) ANTIOXIDANT ANTICORROSION ANTIWEAR/EP TACKINESS (ASHLESS) ANTIOXIDANT ANTICORROSION ANTIWEAR/EP TACKINESS (ASHLESS) RAPE SEED OIL/ POLYMER LI-/CA- 12-0H-STEARATE IN SITU MANUF. OPEN KETTLE ANTIOXIDANT ANTICORROSION TACKINESS (ASHLESSI C -25 TO +130-35 TO +120-20 TO + 110-15 TO +90 WORKING-TEMPERATURE- RANGE APPLICATION AREAS MULTI-PURPOSE MULTIPURPOSE CHASSIS OF TRUCKS AGRICULTURAL. MACHINERY SEAL GREASE IN TUNNEL CONSTR. EQUIPMENT AGRICULTURAL MACHINERY Figure 10: Low temperature consistency vs. time EUROGREASE 2 april/may/june 2013 15

Figure 11: Dynamic oxidation test, equipment Figure 12: Dynamic oxidation test, results Figure 13 / 14: Tunnel excavating and construction machine Figure 15 / 16: Railroad, wheel flange lubrication 16 EUROGREASE 2 april/may/june 2013

Figure 17 / 18: Waste water purification plant and hydro-electric power plant Figure 19 / 20: Centralized lubrication systems on trucks Figure 21 / 22: Forestry applications Figure 23 / 24: Construction machinery EUROGREASE 2 april/may/june 2013 17

2013 ELGI AGM 25 th Anniversary

2013 ELGI AGM 25 th Anniversary

2013 ELGI AGM 25 th Anniversary

2013 ELGI AGM 25 th Anniversary

2011 NLGI Grease Production Survey Presented at the 25 th ELGI Annual General Meeting Amsterdam, The Netherlands April 2013 Chuck Coe Grease Technology Solutions LLC Manassas - USA chuckcoe@grease-tech.com Chuck Coe holds a BS 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 2009. He is NLGI President and is the Grease Education Course Chair of STLE. 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), and the John A. Bellanti Memorial Meritorious Service Award (2012) from NLGI. Abstract The NLGI Grease Production Survey continues to be the single most comprehensive global report on lubricating grease production. It tabulates the global production of grease providing a snapshot of growth by thickener type and base oil type, organized by geographic region of the world. Reporting of grease production by base fluid type was added for the 2010 survey on a probationary basis. This format was continued for the 2011 survey due the excellent response from members of the institute, and will be continued for the 2012 survey as well. This paper will provide a summary overview of the key results and trends from the completed 2011 production survey, as well as an early glimpse at preliminary results from the 2012 survey, which will be published in July, 2013. Introduction Lubricating grease production data is solicited on an annual basis from every known grease manufacturer in the world. Production is requested by thickener type, and since 2010, also by base oil type. Participation is voluntary, and therefore does not include 100% of grease producers. NLGI feels the survey does represent the vast majority of production, probably well in excess of 80% of the world s production. The annual survey report shows data from the year of the survey and the three preceding years. Since the exact same companies do not participate each and every year, the year-to-year trends can be misleading. It is always best to view the data over at least a three to four year period. On a global basis and for regions where there are enough participants to protect individual company s data sufficiently (North America and Europe), comparative data is reported for companies who participated in each of the four reported years, providing a more accurate trend analysis. Overview of 2011 results The global economy continues to show at best a slow recovery in the grease industry in 2011, compared to 2010. Reported worldwide production for 2011 was nearly 1.1 million metric tons (Table 1). This is 10432MT or nearly 1% above 2010 reported production. However, on a comparative basis (companies reporting in all four years), production was actually down by almost 1% from 2010. This discrepancy is primarily the result of the addition of 14 new participants in 2011 compared to 2010. 22 EUROGREASE 2 april/may/june 2013

Region Table 1 2011 Grease Production Survey Statistics Number of Companies Providing Production Data Reported Number Of Grease Plants* Total Lubricating Grease Reported (MT) North America 37 44 220,757 Europe 42 43 186,338 Caribbean, Central & South America 9 11 35,405 Africa & Middle East 5 5 28,858 India & Indian Subcontinent 14 22 86,716 Japan 17 19 76,768 Pacific & South East Asia 7 11 66,612 PRC 31 31 379,641 TOTAL 162 186 1,081,095 In the second year of reporting, production by base oil type was reported by 80% of companies reporting production by thickener type, which was an increase from 70% in 2010 (Figure 1). Some companies are unwilling to report production by base oil type, either viewing it as proprietary or finding it too difficult to provide. Figure 1 Analysis by region Total reported production by region is shown in Figure 2. On a comparative basis, most regions reported higher production volumes in 2011 (Figure 3). Exceptions were Africa & Middle East, and India & Indian Subcontinent, which both had fewer participants than in 2010, so are not truly comparative. Also noteworthy was a 7% decline in reported production from Peoples Republic of China, which followed 2010 s 27% increase over 2009. The decline in reported production from PRC more than offset reported growth in NA and EU. EUROGREASE 2 april/may/june 2013 23

Figure 2 Figure 3 Analysis by thickener type Total production by thickener type is shown in Figure 4. Lithium thickener production continues to be the most significant volume of production, with over 814 thousand metric tons reported. 76% is lithium soap and 24% is lithium complex soap (Figure 5). There continues to be a trend of increasing lithium complex production at the expense of lithium soap greases. Figure 4 2011 Grease Production - By Thickener Type 5% 4% 3% 2% 10% 1% 75% Lithium Calcium PolyUrea Aluminum Other Clay Sodium 24 EUROGREASE 2 april/may/june 2013

Figure 5 Calcium thickener production remained at about 10% of total production, but the multi-year trend is a slow decline from 2006 through 2011 (Figure 6). Calcium sulfonate grew 34% from 2010, to over 20 thousand metric tons. Hydrated calcium thickener production rebounded slightly from 2010, but shows a continuing declining trend. Figure 6 Calcium Thickened Grease Thousand MT 140 120 100 80 60 40 20 0 2006 2007 2008 2009 2010 2011 Ca-Hydrated Ca-Anhydrous Ca-Sulfonate Ca-X Total Ca Polyurea grease production held fairly steady at about 5% of total reported production (Figure 7). China and Japan showed declines, which were offset by reported growth in North America and Europe. Figure 7 Polyurea Thickened Grease Metric Tons 60000 50000 40000 30000 20000 10000 0 2006 2007 2008 2009 2010 2011 MT 43979 46347 52306 40611 53632 56342 EUROGREASE 2 april/may/june 2013 25

Analysis by base oil type Not unexpectedly, grease production is largely based on mineral base oil, with nearly 92% of reported production (Figure 8). Synthetic and semi-synthetic production each showed nearly 4% of the total, while bio-based production represents less than 1% of the total. Any comparison to 2010 reporting by base oil type is risky at this point, with only two consecutive years of reporting. Figure 8 Total All Countries, % 3,811909768 3,716807938 0,783932412 mineral synthetic semi-synthetic bio-based 91,68734988 2012 Survey preview The 2012 production survey is underway, and the final report will be available in June 2013. As of the beginning of April, over 80% of last year s participating companies had submitted 2012 data, which is well ahead of similar reporting at this time last year. Additionally, reporting by base oil type is running at about 90% of participants, which is 10% ahead of the final result for 2011. There have already been 7 new participants for 2012 compared to 2010. 26 EUROGREASE 2 april/may/june 2013

Main Bearing Lubrication for Wind Turbines A Systematic Approach towards Grease Selection Presented at the 25 th ELGI Annual General Meeting 2013 Amsterdam The Netherlands David A. Pierman The Timken Company Canton, OH - U.S.A. dave.pierman@timken.com David has 30 years of lubrication related experience in technology, industrial applications, and tribology at the Timken Company and BP Oil. M.S. in Chemistry from Case Western Reserve University in Cleveland, Ohio and hold (3) patents in various technologies including grease development. He wrote numerous articles for trade magazines on lubrication and is an active member of NLGI, ELGI, and STLE. Abstract Bearing companies are frequently asked for wind turbine main shaft bearing grease recommendations. This is typically not a straightforward request because potential wind turbine main bearing greases can vary significantly in properties depending on the supplier. Furthermore, certain grease properties are difficult to compare due to the availability of multiple test methods targeted at quantifying a specific property or characteristic. A comprehensive survey of grease performance characteristics for wind turbine main shaft bearing applications was prepared in this study by generating a data matrix based on available main bearing engineering data, lubricant supplier information, and wind turbine operator feedback. A goal was to include both application-relevant and standardized test data to allow head-to-head comparisons among the various grease candidates. The data are examined for trends that allow for grease recommendations specific to different environments. For example, an off-shore environment requires grease with better seawater corrosion protection than do on-shore applications. This work employed standardized test methods to evaluate wear, lube film thickness, bearing functional/spin test, corrosion protection, fretting wear protection, low temperature torque, oil separation properties, pumpability, EP (Extreme Pressure) properties, and shear stability. Both in-house and independent laboratories generated test data on a total of ten greases with varying base oil viscosities, NLGI (National Lubricating Grease Institute) grades, and additive packages. An approach using DFSS HoQ (Design for Six Sigma House of Quality) methodologies was used to determine rankings of the greases based on the application and customer requirements, as well as results of subsequent testing. The data were analyzed using Pugh-type diagrams assuming six different wind turbine environments. The greases were then scored 28 EUROGREASE 2 april/may/june 2013

for each condition by their test results and ranked. Introduction Increasing demands on wind turbine plants require lubricants that are optimized for the application requirements inherent in these gear and bearing applications. Diverse conditions in wind turbine main shaft bearings include slow bearing speed, wind induced vibrations, saltwater mist from off-shore locations, and a wide climate range. Optimized greases are required for sets of very specific operating conditions that depend greatly on the turbine location. In most cases, general purpose greases will not address all of the application requirements. Surveying the grease products currently used for main bearing applications revealed a mix of ISO base oil types (mineral or synthetic), base oil viscosity grades, thickener types, and NLGI (National Lubricating Grease Institute) consistency grades. Grease test properties addressing the application requirements such as fretting wear, pumpability, and corrosion resistance were not always reported in commercial literature, and if they were, the test results were not always comparable due to the use of customized test methods. In this paper, main bearing grease products were subjected to an extensive test program based on main bearing application requirements. Statistical methods were applied to rank the performance of each grease overall, and to quantify the positive and negative attributes of each grease. No single grease in this study possessed fully optimized properties for every application environment, so grease selection for a particular wind turbine main bearing is subject to specific application environment and property requirements. Experimental Table 1 shows the ten greases that were evaluated. Eight of these greases were commercial products recommended for use in wind turbine main bearing applications and two of the greases were experimental products. All of the greases were lithium-based, either as lithium soap or lithium complex, and were further categorized by their grade, base oil viscosity class, and type of base oil (synthetic or mineral). A single letter from A-G designated each grease category. Repeating categories contain a number after the category letter. For example, greases B1, B2, B3, and B4 are all similar in grade, base oil viscosity classification, and type of base oil but have different additive packages that can change the test properties. Table 1 Grease Data Grease Property Grease A1 Grease B1 Grease C1 Grease D1 Grease E1 Grease F1 Grease B2 Grease B3 Grease G1 Grease B4 # 1 2 3 4 5 6 7 8 9 10 Thickener Li Base Li Base Li Base Li Base Li Base Li Base Li Base Li Base Li Base Li Base Grease NLGI Grade 1 2 1 2 0 2 2 2 1 2 Base Oil Type Syn Syn Mineral Mineral Syn Syn Syn Syn Syn Syn Viscosity @40 C, cst L H H M H M H H H H Vis Class, cst 150 L 151-299 M 300 H EUROGREASE 2 april/may/june 2013 29

The ten grease characteristics identified as significant for a main bearing application are proposed as follows: 1. Lube film thickness Traditionally, lube film thickness is associated with the base oil of the grease. However, grease thickeners and polymers in a grease can work synergistically to improve the grease film thickness. 2. Oil separation The amount of oil released from a grease for EHL (Elastohydrodynamic Lubrication) film formation. Too much oil release can deplete the thickener of oil over time and leak from the seal resulting in the grease getting heavier and heavier. Too little oil release results in dry rollers and raceways. Oil bleed is also thickener type-dependant. 3. Bearing wear behaviour Extremely low rotational speeds of a wind turbine main bearing (20-30 rpm) can result in bearing wear (peeling or micropitting) if there is insufficient lube film. 4. Spin test Proper grease migration within the bearing cavity is important in the lubrication of a wind turbine main bearing. Grease should be evenly distributed and the rollers and raceways should show a visible lube film after bearing spin testing. 5. EP properties EP properties of a lubricant are important to minimize wear in low speed applications by creating a sacrificial surface layer. 6. Grease pumpability Grease pumpability is critical in cold temperatures, especially in centralized grease systems. 7. Shear stability A grease must be able to maintain its consistency under shear. Excess grease softening can cause grease leakage. 8. Low temperature torque The ability of the grease to migrate within the bearing, especially in cold climate. Lack of grease can cause dry raceways. 9. Corrosion protection The ability of the grease to prevent corrosion especially in off-shore applications where salt water mist is present. 10. Fretting wear protection The ability of the grease to protect against fretting wear. Fretting wear can be generated in the wind turbine main bearing during shipment and by wind induced oscillation when the wind turbine is idle. Test procedures and test data Lube film thickness, WAM6 Horseshoe Measurement Lubricant film formation capability of wind energy greases was measured using an AChILES optical EHL (elastohydrodynamic lubrication) apparatus on a WAM6 (Wedeven Associates Machine) ball on disk tribometer. All measurements were made using grease at room temperature with a test load of 40 N. To evaluate the fully-flooded lubricant supply condition, five measurements were performed at each of three speeds: 40 mm/s (0.04 m/s), 50 mm/s (0.05 m/s), 60 mm/s (0.06 m/s). The central film thickness for each of the five measurements was recorded at each speed. A total of fifteen measurements were collected for each grease. For starved lubrication conditions, five measurements were made at each of two speeds: 60 mm/s (0.06 m/s), 100 mm/s (0.10 m/s). The central and minimum film thickness for each of the five measurements was recorded at each speed after 30 seconds of running without spreading the grease back into the track. Oil Separation DIN 51817, 7 days @40 C A cylindrical column of grease resting on a metal gauze cone is subjected to a fixed pressure in excess of the hydrostatic pressure of the grease. The quantity of oil separated through the gauze after standing for 42 h or 168 h at 40 C is taken as a measure of the stability of the 30 EUROGREASE 2 april/may/june 2013

grease towards oil separation during storage. The oil separation is reported as a percentage. cut-off. Test samples are removed, weighed, and photographed. Wear behaviour (report bearing test) DIN 518 19 FE8 The FE8 test rig was designed to simulate the tribological systems of real-world applications. Grease testing follows test Condition 1, although several variations of the test can be run. Condition 1 uses taper roller bearings (K 530048) run at 7.5 rpm under an axial load of 80 kn. Two new pre-weighed test bearings are packed with grease and run at a self-induced temperature for 500 hours. During the test run, the friction moment of both bearings and the outer ring temperatures are recorded. Wear of the parts is determined after the run. The amount of wear is statistically evaluated according to the statistical Weibull failure distribution diagram and the 10 percent and 50 percent rolling element set wear values in mg (V10 and V50, respectively) are reported. The friction moment at start, 20, 100, and 500 hours and the steady state and maximum temperatures are also reported. Wear mass is recorded in milligrams. Grease pumpability Pumpability is defined as the pressure which is necessary to achieve a flow rate of 10g/min @ - 25 C when the grease is forced through a pipe 1m in length and 7mm in diameter. ASTM D217A shear stability Grease consistency is measured with a penetrometer by working the grease 60x and 100,000x and recording the penetration difference. This is a measure of shear stability. (+) is softening, (-) is hardening. Low temperature torque (-40 C), ASTM D1478 This test method evaluates the extent to which grease retards the rotation of a slow-speed ball bearing by measuring starting and running torques at -40 C. It is the torque required to prevent rotation at 1 rpm. Wear mass is reported in milligrams. Spin test (Timken in-house) A 1.9m outer diameter two-row TRB (tapered roller bearing) is charged with a 30% fill of test grease and run 24 hours at 10 rpm followed by 48 hours at 20 rpm using a non-contact seal. Torque and temperature are monitored followed by bearing disassembly and inspection. Running torque and grease distribution are reported as comments. Falex block on ring Fretting & EP properties The Falex block on ring test is run at a load of a 4480 N (1000 lb), an oscillation frequency of 3.33 Hz (200 cpm), and a stroke of 0.087 radians (5 ). Only 0.05 g of grease is applied to the contact between the ring and the block prior to load-up and test initiation. The test is run for 22 hours or until the 672 N (150 lb) friction force Corrosion Protection Emcor Test DIN 51 802/ASTM 6138 The Emcor test measures the ability of grease to protect a bearing against corrosion in the presence of water. Two sets of grease-coated bearings per station are partially immersed in water and rotated at a speed of 80 rpm in a sequence of running and resting periods. At the end of the test, the raceways of the bearing outer rings are inspected for rust. Rust ratings range from 0-5 with (0) being no rust and (5) containing 10% rust. Fretting Wear Protection ASTM D4170 (Fafnir) Two thrust type bearings lubricated with grease are loaded to 550 pounds force and oscillated through a 12 arc at 1800 cycles per minute for 22 hours at room temperature. The fretting wear is the average weight loss of the two bearings. EUROGREASE 2 april/may/june 2013 31

Table 2 Test Data Grease Product Grease A1 Grease B1 Grease C1 Grease D1 Grease E1 Grease F1 Grease B2 Grease B3 Grease G1 Grease B4 Characteristics 1 2 3 4 5 6 7 8 9 10 Thickener Li Base Li Base Li Base Li Base Li Base Li Base Li Base Li Base Li Base Li Base Grade 1 2 1 2 0 2 2 2 1 2 Base Oil Type Syn Syn Mineral Mineral Syn Syn Syn Syn Syn Syn Viscosity (cst), 40 C L H H M H M H H H H Tests Oil Separation DIN 51 817, 7 days @ 40 C, static, % 4.0 2.0 3.2 3.5 5.5 2.0 2.0 1.5 2.8 3.4 Low Temperature Torque (-40 C), ASTM D1478 Starting/Running, g-cm 4498/546 3146/793 >35,000 >35,000 2516/1040 6450/1505 9,000/2944 10,700/3480 2938/1209 7046/832 Corrosion Protection Emcore Test DIN 51 802 ASTM 6138, (0,0) 1% (0,0) 1% (0,0) DI Water (1,1) 100% (0,0) DI (0,0) DI (0,0) DI Water (0,0) 1% NaCl rating at DI water/seawater?1 DI Water NaCl NaCl Seawater Water Water (0,0) DI Water (0,0) DI Water (1,2) 1% NaCl (1,2) 3% NaCl Fretting Wear Protection ASTM D4170 (Fafnir), 25 C, mg wt loss 1.3 1.9 2.8 5.7 0.9 25.5 22.2 56.8 2.45 0.98 518 19, FE8, 80kN, 500h, mg wear 32.5 2 85 42.5 NA 45.2 45.5 54.4 129 3 Spin Test (ft-lbs) 850 Pass 255 Pass (rollers dry) 1000 Pass Pass NA NA Pass >1500 Fail 800 good coverage 750 dry rollers Falex, wt loss, mg 0.7 5.5 0.6 0.58 1.00 0.58 0.33 1.03 0.26 0.42 Lube Film Thickness (Continuous) 611 291 342 394 337 239 377 554 250 275 Lube Film Thickness (Starved) 704 141 155 168 223 na 162 554 150 180 Pumpability (pressure which is necessary to achieve a flow rate of 10g/min @ -25 C), bar 11 28 24 80 na na 20 75 21 40 ASTM D217A Shear Stability W/100,000X, % change 10 9 10 14 1.2 8.9 9.5 0.3 4 12.2 Test Results Rating Good 6 Average 3 Poor 1 Results and discussion A list of grease data and test results is shown in Table 2 Data were analyzed by the use of DFSS HoQ (Design for Six Sigma House of Quality) and were set up in two steps. Step 1 was to define the engineering parameters. These are listed in Tables 3a-3c column A. Then the parameters were assigned a weight factor depending on their importance according to six different environmental conditions. Step 2 involved rating of each grease against a weighted test value (Tables 4a-4c). Step 1: HoQ1 Engineering Parameter Vs Test: Tables 3a- 3c The first step in the HOQ diagram process was to define the engineering parameters. These are listed in HoQ1 Tables 3a-3c column A. The parameters were assigned a weight factor depending on their importance. The weights were based on the following rating system: Rating Significance 1 Slightly Important 3 Moderately Important 6 Strongly Important Six different environmental conditions were evaluated this way which include: (1) Onshore Normal Climate Wt., (2) Onshore Cold Climate Wt., (3) Onshore Hot Climate Wt., (4) Offshore Normal Climate Wt., (5) Offshore Cold Climate Wt. and (6) Offshore Hot Climate Wt. These conditions were selected based on known environmental combinations. However, any given application may not necessarily fit into any of these categories. Each engineer must decide if the weighting is appropriate for their given application. The tests were then listed along the top (row 1) and a rating was assigned to each parameter/test cell. This rating reflects how significant the test evaluates the engineering parameter. Then each rating is multiplied by its parameter weight and totalled for each test. This produces a test weight to be used in the HoQ2 test vs. grease product diagram (tables 4a 4c Column B) where the weighted test value is rated for each grease. 32 EUROGREASE 2 april/may/june 2013

Step 2: HoQ2 Test Vs Grease: Tables 4a 4c Test results for each grease are rated by their test values which are colour coded in Table 1: Rating Significance 1 Deficient test value 3 Average test value 6 Superior test value The test result rating is then multiplied by its test weight and a total is tabulated for each grease. Final rankings were sorted below each total. The test rating process involved reviewing each test and determining what constitutes an average test value, a deficient test value, and a superior test value. Obviously, this was not an easy task and was very subjective. Table 3 shows the test result ranges and rankings. Table 3 Test result rankings Tests Result Range Deficient test value Average test value Superior test value Oil Separation DIN 51 817, 7 days @ 40 C, static, % 1.5-5.5 <2.5 or >4.0 NA 2.5-4.0 Low Temperature Torque (-40 C), ASTM D1478 Running, g-cm 546-3480 >2500 1250-2500 <1250 Corrosion Protection Emcor Test DIN 51 802 ASTM 6138, rating at DI water/seawater 1 DI Water-(0,0) 1% NaCl (0,0), DI Water or less (0,0) DI Water (0,0) 1% NaCl or better Fretting Wear Protection ASTM D4170 (Fafnir), 25 C, mg wt loss 0.9-56.8 >10 5-10 <5 Wear Behaviour (K 53048) DIN 518 19, FE8, 80kN, 500h, mg wear 2-129 >50 36-50 <35 Spin Test (ft-lbs), Grease distribution, comment only NA Dry Rollers and/or high torque Adequate lube film and distribution, medium torque Good lube film and grease distribution Falex, wt loss, mg 0.26-5.5 >3 1-3 <1 Lube Film Thickness (Continuous), normalized 239-611 250 251-400 >400 Lube Film Thickness (Starved), normalized 141-704 <200 201-400 >400 Pumpability (pressure which is necessary to achieve a flow rate of 10g/min @ -25 C), bar 1-80 >50 26-50 <25 ASTM D217A Shear Stability W/100,000X, % change 0.3-14 >10 5-10 <5 Test Results Rating Rating Superior test value 6 Average test value 3 Deficient test value 1 EUROGREASE 2 april/may/june 2013 33

Oil bleed is dependent on thickener type and grease grade which made it difficult to apply ratings. However, for this test work, oil bleed of 2.5-4.0% was considered optimal for the lithium based greases tested. Oil bleed <2.5% was less desirable as observed in several of the spin tests exhibiting dry rollers. Oil bleed >4.0% was also considered less desirable due to potential leakage. From the existing data, the following observations and rankings were made from HoQ diagrams: Grease A1 (#1) ranked 1 st in all environmental conditions. One of the biggest contributors to this ranking was the lube film thickness test which was the highest among the greases tested. Although the base oil viscosity class was L, the overall lube film thickness appeared greater than the base oil by itself. Grease B4 (#10) ranked 2 nd in all environmental conditions. This was an experimental grease which exhibited excellent anti-fretting and antiwear behaviour but the rollers still appeared dry in the spin test. The dry rollers may not be an issue considering that this formulation does contain EP additives which can increase lube film thickness, but this has not been quantified. Grease G1 (#9) ranked 3 rd in all environmental conditions. This was an experimental grease exhibiting good anti-fretting and low temperature torque properties but pumpability and wear behaviour on the FE8 test was poor. The spin test showed good migration and oil film. Grease E1 (#5) ranked 4th in all environmental conditions. Grease E1 had one of the lowest low temperature torque values and excellent antifretting properties. Its primary disadvantage is being a grade 0 which is somewhat flowable thus the potential for grease leakage. Grease B1 (#2) and Grease C1 (#3) ranked 5 th and 6 th depending on the environmental condition. Both greases had high marks in antifretting and anti-corrosion properties. The biggest disadvantage for the C1 grease is its mineral base oil which limits low temperature torque (grease is considered frozen at -40 C) and excessive wear on the FE8 test. Grease B1 exhibited dry rollers in the spin test. Grease B3 (#8) rated 7 th overall. Although the excellent shear stability and lube film thickness were positive, the poor anti-fretting and grease migration properties pulled the ranking down. Greases D1 (#4) and B2 (#7) were middle of the road in properties ranking 8 th and 9 th respectively. The anti-fretting properties of these two greases were average- to-poor. Finally Grease F1 (#6) ranked 10 th exhibiting average to below average performance properties on most of the tests with very poor anti-fretting characteristics. Spin test results and discussion Most, but not all, of the grease samples were subjected to a full scale spin test. In this test, a single test bearing (1.9 meter) was used to perform extended spin tests. Torque and temperature were recorded throughout the duration of the test. These differed greatly between the grease samples. The bearings were also inspected after the test for a subjective review of film thickness and grease distribution. One of the results of the spin test was the visual appearance of oil/grease on the raceways after testing. The study demonstrated positive results if the visual appearance correlated directly with oil separation. It was also determined to not include the spin test visual results in order not to double count the same factor. Additionally, there is some level of subjectivity to the spin test raceway wetting results, while the oil separation tests are more objective. A data acquisition device plotted torque, temperature, and speed. Post testing includes removing a part of the cage and several rollers to observe grease migration and lube film generation in the bearing contact areas. An example of the torque and temperature results are shown in Figure 1for grease B1 It was difficult to rank the success of the torque and temperature results of the tests. High torque itself it not necessarily an issue, as long as the grease provides good lubrication properties. Conversely, low torque may not be beneficial, especially if the grease results in relatively dry raceways. Grease B1 showed the lowest torque and average temperature. Grease B3 had the highest torque and highest temperature as shown in Figure 2. All greases showed 34 EUROGREASE 2 april/may/june 2013

reasonable grease distribution and raceway wetting except for the Greases B1 and B4 which tended to give dryer raceways and roller bodies. Summary and conclusions Eight commercial main bearing wind greases and two non-commercial main bearing grease candidates were evaluated for their standard properties such as low temperature torque, anticorrosion, anti-wear, and anti-fretting properties as well as Timken in-house tests for the spin test, lube film thickness, and EP properties. Some of these properties varied greatly depending on the grease. The data was analyzed by the use of HoQ diagrams and a grease ranking was documented. A review of all of the environmental conditions showed only subtle differences in grease ranking, using the process documented here. For example, only for the off-shore platforms in normal and hot climate conditions were there slight differences between greases B1 and C1. Also, greases B1-B4 which had similar properties such as grease thickener (Lithium Complex), grease grade, viscosity class, and base oil type did not show the same performance characteristics in the test data. For example, grease B1 has much better antifretting properties than grease B3. The ranking is summarized from the data as follows: 1 Grease A1 2 Grease B4 3 Grease G1 4 Grease E1 5 Grease B1 6 Grease C1 7 Grease B3 8 Grease D1 9 Grease B2 10 Grease F1 No particular grease in this study possesses fully optimized properties, making grease selection dependent on the properties desired for each set of application conditions. Table 3a: HOQ1 Diagram: Engineering Parameter vs. Test EUROGREASE 2 april/may/june 2013 35

Table 3b: HOQ1 Diagram: Engineering Parameter vs. Test Table 3c: HOQ1 Diagram: Engineering Parameter vs. Test 36 EUROGREASE 2 april/may/june 2013

Table 4a: HOQ2 Diagram: Grease Test vs. Grease Product Table 4b: HOQ2 Diagram: Grease Test vs. Grease Product EUROGREASE 2 april/may/june 2013 37

Table 4c: HOQ2 Diagram: Grease Test vs. Grease Product Figure 1 Grease B1 Spin Test Data Figure 2 Grease B3 Spin Test 38 EUROGREASE 2 april/may/june 2013

Independent Union of the European Lubricants Industry Union Indépendante de l Industrie Européenne deslubrifiants Congress 2013 Annual Congress of the European Lubricants Industry 23-25 October 2013 - Brussels Registrations are now open! www.ueil.org OPT-JPremy In cooperation with Sponsors: UEIL Rue du Luxembourg, 22-24 B-1000 Brussels Tel: +32 2 761 66 85 Fax: +32 2 213 13 63 email: info@ueil.org

Forthcoming Meetings ELGI Board Meeting October 2013 ELGI Board Meeting ELGI Working Groups 16 June 2013 Grease Cleanliness WG Meeting - NLGI Annual Meeting 16 June 2013 Grease Shelf Life WG Meeting NLGI - Annual Meeting 16 June 2013 Food Grade Lubricants WG Meeting - NLGI Annual Meeting 16 June 2013 Bio-Based Greases WG Meeting - NLGI Annual Meeting 10 September 2013 Railway Lubricants Task Force Meeting (TBA) 23-25 October 2013 Food Grade Lubricants WG Meeting during UEIL Conference Brussels (TBA) 25 th November 2013 Grease Cleanliness WG Meeting - Amsterdam 25 th November 2013 Test Methods & Rheology WG Meeting - Amsterdam 26 th November 2013 Bio-Based Greases WG Meeting - Amsterdam 26 th November 2013 Railway Lubricants WG Meeting - Amsterdam Other Meetings 2013 15-18 June 2013 NLGI 80 th Annual Meeting Tucson, Arizona, USA. www.nlgi.org / nlgi@nlgi.org 26-27 June 2013 ERGTCEF Meetings Amsterdam. kathy@calebgroup.net andreas.dodos@eldons.gr 26-27 June 2013 ICIS 7 th Asian Base Oils & Lubricants Conference Singapore. www.icisconference.com/asianbaseoils 3-6 September 2013 Oil and Gas Conference and Exhibition. Aberdeen, UK www.offshore-europe.co.uk 4-6 September 2013 Leeds-Lyon Symposium on Tribology. Lyon France. leeds-lyon@insa-lyon.fr 10 September 2013 RLWG Task Force Amsterdam. carol@elgi.demon.nl 8-13 September 2013 5 th World Tribology Congress Torino, Italy. www.wtc2013.it 15-19September 2013 SAE 11 th International Conference on Engines & Vehicles. Capri, Italy 18-19 September 2013 European Base Oils & Lubricants Summit. Budapest, Hungary. cwilliams@acieu.net 25-27 September 2013 Argus Asian Bitumen 2013. ellen.chan@argusmedia.com / www.argusmedia.com 5-8 October 2013 ILMA Annual Meeting. Texas, USA. www.ilma.org 8-9 October 2013 ICIS 10 th Middle Eastern Base Oils & Lubricants Conference. Dubai, United Arab Emirates 18 October 2013 XI International Forum Russian Oil & Gas Industry. Moscow 23-25 October 2013 2013 UEIL Annual Congress of the European Lubricants Industry Brussels. www.ueil.org / info@ueil.org 23-25 October 2013 TBA ELGI Food Grade Lubricants Meeting. a.adam@fragol.de 6 November 2013 UKLA Annual Dinner London UK. enquiries@ukla.org.uk / www.ukla.org.uk 6-7 November 2013 ICIS 2 nd African Base Oils & Lubricants Conference. Cape Town, South Africa 12-15 November 2013 IV Moscow International Lubricants Week. Moscow 25 November 2013 25 November 2013 26 November 2013 26 November 2013 Grease Cleanliness WG Meeting Test Methods & Rheology WG Meeting Bio-Based Greases WG Meeting Railway Lubricants WG Meeting Amsterdam: Further details carol@elgi.demon.nl 5-6 December 2013 ICIS 9 th American Base Oils & Lubricants Conference. New Jersey, USA 2014 21-23 January 2014 TAE 19 th International Colloquium Tribology Industrial and Automotive Lubrication. Stuttgart/Ostfildern, Germany www.tae.de/tribology 17-19 February 2014 International Petroleum Week. London, UK www.energyinst.org/events/ip-week 20-21 February 2014 ICIS 18 th World Base Oils & Lubricants Conference. London, UK 1-2 April 2014 UNITI Mineral Oil Technology Congress. Stuttgart, Germany leber@uniti.de / www.uniti.de 26-29 April 2014 26 th ELGI Annual General Meeting. Dubrovnik Croatia www.elgi.org 18-22 May 2014 69 th STLE Annual Meeting. www.stle.org. Mhedland@stle.org 14-17 June 2014 NLGI 81 st Annual Meeting. Palm Beach Gardens, FL, USA nlgi@nlgi.org / www.nlgi.org 18-21 October 2014 ILMA Annual Meeting. California, USA. www.ilma.org 40 EUROGREASE 2 april/may/june 2013

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