NLGI 2001, 68th Annual Meeting, October 27 31, Palm Beach Florida

Need quick, reliable and proactive information on remaining grease life? Are you looking for a portable method, measuring the remaining useful life of used greases?
The answer to your question is the RULER, Remaining Useful Life Evaluation Routine, and portable equipment. A test method that covers the determination of Remaining Antioxidant concentration in used greases by the portable RULER technology.

Why and what is Remaining Useful Grease Life?

During their use in the lubrication systems, lubricating greases experience oxidative stresses, which degrade the chemical composition of the oils basestock and deplete the oils additive package. It is well known that to inhibit the oxidation of the oil, antioxidants are added to the oils basestock. The remaining useful life of a lubricant is the length of an operating time from when a lubricant is sampled, until the antioxidants are depleted, allowing large changes in the basestocks physical properties to occur due to oxidation. If a grease is used past the end of its useful life, excessive degradation can occur, resulting in component wear and eventually equipment malfunction. The RULER will give the ability to every user of grease to predict the remaining useful grease life, which would eliminate the need for scheduled changes, providing savings in operating costs to various types of equipment users. It could also be used to identify lubricants being degraded at an accelerated rate by abnormally operating equipments (e.g. bearings). Such identification before equipment malfunction would provide additional savings to equipment users.

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NLGI 2001, 68th Annual Meeting, October 27 31, Palm Beach Florida

The graph below represents the depletion of antioxidants, in function of the remaining grease life, and physico-chemical characteristics as TAN, and oxidation products (detection by FTIR) buildup.

How to use the RULER

RULER test procedures Select Small Grease Sample Size range of 50 400 mg grease Spread out on inside of glass vial Shake & Mix for approx. 1 minute of time (Vortex mixer) Insert probe and perform tests Total time of 17 seconds Save & record RUL% data o % Remaining grease life o as a comparison between new and used grease

RULER Test Solution vials with grease before and after dissolving

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NLGI 2001, 68th Annual Meeting, October 27 31, Palm Beach Florida

RULER Test advantages

easy sample preparation (50-200l )

The RULER test procedures have the major advantage that no separate, and timeconsuming extraction phase is necessary. Only small grease samples are necessary

fast on-site analysis

The total time for performing the RULER test procedures, will take approximately 4-6 minutes.

simple to operate

The RULER will guide you through the operating procedures, powered by Windows CE

no hazardous chemicals for extraction

You will avoid to use and disposal costs of environmental unfriendly solvent, which are necessary to extract the antioxidants out of the grease structure.

readily available consumables

For quick and repeatable analysis

correlation w ith R BOT, TOST, DSC, FTIR

see further at chapter - publications Area of application where for using the RULER? On all type of greases, which contain at least 1 type of antioxidant, covering EP-type of greases, middle to high temperature greases, with both mineral and synthetic base oils. Different research programs (see SKF paper, ELGI 2001) have shown excellent detection capabilities of the RULER for a wide range of antioxidants: ZDDP

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NLGI 2001, 68th Annual Meeting, October 27 31, Palm Beach Florida

Amines class of antioxidants

Phenolic class of antioxidants

RULER Test equipment RULER Package, Ref. 320S-200 This package also includes a handy carrying case for instrument & supplies for easy transport. S S S S S S RULER instrument CE320 with docking cradle, cable and communication software R-DMS Software (RULER Data Management Software) Carrying case for instrument and accessories Micropipettor (200L) with tips Cleaning material: alcohol pads, tissue wipes CD-ROM with RULER interactive operation manual

Note: The 200L micropipettor is a standard size pipettor used for most lubricating oils. Lower sizes micropipettors are also available for oils containing higher levels of antioxidants.
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RULER Features o Patented electrochemical technique o Patented color-coded test solutions formulated for the type of oil or lubricant being tested o Compact and completely portable palm unit o Easy to use software Powered by Windows CE o Easy to operate super flex touch screen controls o 320 x 240 pixels LCD back-lighted touch screen o Touch screen with Automatic contrast temperature compensation o Unit can store sample data for over 100 tests o Quick wireless Infrared Link to Personal Computers o Easy Drop-In Communication and charging cradle o Long Life Li-Ion battery with Backup reserve o Integrated charge status and low-battery indicator with Intelligent fast charge o Custom durable Screw-on probe for test solution vials o Palm unit equipped with Intel, Strong Arm SA 1100, 190 MHz, 32 bit RISC processor o Memory: 16 Meg DRAM and 16 Meg of NAND Memory o Fully tested for harsh and industrial environment

RULER Specifications

Physical characteristics Size 60 mm (H) x 104 mm (W) x 248 mm (L) Weight 840 g Electrical Circuitry designed to optimize the use of voltammetry in a 0.0 1.7 Volt range for lubricants Power Supply 1 rechargeable Lithium-ion battery pack Separate rechargeable lithium-manganese backup battery AC Adaptor 120 VAC 60 Hz or 220 VAC 50/60 Hz Communication one high speed 4MBPS IrDA port on the instrument Standard RS-232 on cradle Temperatures: operating: -30C to +50 C / -22 F to +122F Environmental: Sealed meets IP67 (Immersion),MIL-STD-810E method 506.3 procedure (Rain) and method 512.3 procedure 1 (immersion) / shock Resistant: meets MIL-STD-810E method 561.4 procedure 4, CEI 68-2-32 method 1 Withstand electrostatic Charge (meets EN61000-4-2) Approval: FCC, Class A, CE certification

RULER Test Solutions

The RULER vials (7mL glass vials filled with 1g of sand and 5mL of the specified solution) are pre-packed in a case of 144. RULER solutions are also available as a mixture of different solutions; in your case we could offer a mixture of 72 Green test solutions (for your hydraulic fluids), and 72 Blue test solutions (for your engine oils).

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R-DMS Ruler Data Management Software

R-DMS , is a Windows based software designed for the RULER CE 320. It allows end-users to download RULER field data from the CE320 field unit to desktop software. With R-DMS , the user can mai ntain large databases, trend time-series testing, view multiple tests, and export data to other formats.

Figure :RDMS printout, showing trending graph for multiple grease samples.

Applications : condition monitoring, quality control and research purposes Roller bearing greases (automotive, electrical applications) High-speed train roller bearing greases Actuators power generation (MOV) References SKF European Research Centre Publications 1) Prediction of Remaining Grease Life a new approach and method by linear sweep voltammetry - Paper presented at the ELGI AGM 2001, Bern, May 2001. Albert van den Kommer SKF ERC, Nieuwegein, The Netherlands

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Jo Ameye FLUITEC International, Brussels, Belgium Abstract: This paper presents the results of research program to evaluate and predict the remaining grease life of greases used in deep groove ball bearings. The technique studied in this paper is based on linear sweep voltammetry1, which directly extracts the antioxidants out of the base oil into a working solution. By applying a controlled voltage ramp through the electrode inserted into the diluted grease sample, a current to flow will peak at the oxidation potential of the antioxidant. The height of the peak is related to the concentration of the additive in the solution. The components in a grease are predominantly base fluid containing specifically designed additives, like antioxidants. It is these additives, which provide the lubricants functions and also protect the base fluid from oxidative degradation. In a first step the precision of the voltammetric analysis was tested. Typically antioxidant peaks are detected from zinc dialkyl dithio phosphate, phenolic and amine type of antioxidants. In a second step a series of samples from different oxidation tests, were analysed using voltammetry. The results showed that the antioxidant capacity depleted with time, but that the rate of depletion varied depending on operating conditions. The voltammetric results were correlated to measurements results from other analytical techniques, i.e. High Performance Liquid Chromatography and Fourier Transfer Infra Red Spectroscopy. It is concluded that voltammetry (by mean of the RULER technology)(1) can determine rapidly the effective antioxidant concentration in greases. If the total effective antioxidant capacity depleted rapidly to a low level this could suggest the grease is inappropriate for the equipment particular duty cycle or re-lubrication of bearings is needed.
100 90 80 AO by Area RUL% 70 60 50 40 30 20 10 0 0 250 500 750 1000 Time [hours] 1250 1500 1750
Area RUL Dynamic test Area RUL Static Test Oxidation Static Test Oxidation Dynamic Test

2 1.8 Oxidation level Rox 1.6 1.4 1.2 1 0.8 0.6 0.4 0.2 0

Correlation graph between RULER detection levels for antioxidants, and Oxidation level detected by FTIR on oxidized grease samples.

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Antioxidant Concent and grease oxidation 100 80

AO HPLC indirect

0.75

60

Total AO RULER indirect Total AO RULER direct Oxidation FTIR

0.5

40 20 0
0 240 450
Time [hrs]

0.25

500

750

950

Graph showing correlation between RULER and HPLC for detection of antioxidant concentrations on oxidized grease samples. 2) Remaining Useful Life Measurements of Greases Using Cyclic Voltammetric Method Robert E. Kauffman UDRI, Dayton, Ohio paper presented at STLE Meeting 1994 Abstract - This paper represents the results of a research paper designed to develop a remaining useful life evaluation rig (RULER) for cyclic voltammetric methods for diesel engine oils, automotive engine oils, hydraulic fluids, and greases. The RULER requires less than one milliliter of sample, less than one minute to perform and very little technical expertise. Samples of laboratory-stressed and authentic-used oils, fluids and greases were used in the development of the RULER. The results of this research demonstrate that remaining useful life measurements made by the RULER can be used by oil analysis programs to quantify antioxidants levels of incoming and stored supplies, to predict and extend oil change intervals for normally operating equipment, and to detect abnormally operating equipment prior to malfunction. Laboratory stressed greases To evaluate the capability of the RULER to measure the remaining useful life of greases, a Lithium-complex synthetic grease was oxidized and sampled at 175C. The percentage remaining additive measurements of the stressed samples were plotted vs. stressing time as shown in figure below. The antioxidant designated 1 in the figure depleted during initial oxidation and the antioxidant designated 2 in the figure started to deplete once Antioxidant 1 had been reduced to 60% of its original concentration. Once Antioxidant 1 reached 15% of its original concentration, hairline
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cracks were observed in the grease films indicating accelerated oxidation of the basestock. After 24 hrs of further stressing, the grease became further cracked and started to harden. Other types of greases heated at 150C showed similar relationships between antioxidant depletion and the formation of hairline cracks in the heated grease films.

Authentic used greases To evaluate the capability of the RULER to monitor the antioxidant depletion in actual used greases, used DOD-G-24508A grease samples obtained from the bearings of normally and abnormally operating equipment were analyzed. The voltammograms of the fresh and used DOD-G-24508A greases show in the figures below demonstrate that the RULER is able to detect antioxidant depletion in used greases and the antioxidant depletion appeared to be greater for the abnormally operating equipment. Conclusions on the significance of antioxidant depletion in the grease sample obtained from the abnormally operating equipment can not be made since the maintenance records were not available.

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