ESCIT 2006 ©Ciba Specialty Chemicals Phosphorus Volatility Bench Test ESCIT Meeting August 8 th, 2006 Toyota Technical Center Ann Arbor, MI Presented By ©Ciba Specialty Chemicals

ESCIT 2006 ©Ciba Specialty Chemicals 1.Presentation Objectives 2.Overview of test methods 3.Assessment of Phosphorus Volatility  Realistic testing Procedures  Results of bench tests 4.Applicability and Correlation  Catalyst Performance Evaluation  Results PEI Summary & Future Work  Larger sampling of chemistries  Industry Collaboration Topics

ESCIT 2006 ©Ciba Specialty Chemicals Presentation Objectives Introduce and offer the industry a potential new test for evaluating phosphorus volatilization in engine oils Demonstrate the ability to differentiate phosphorous depletion (catalyst poisoning) Gain industry support for further evaluation

ESCIT 2006 ©Ciba Specialty Chemicals Assessment of P volatility In our previous publications, several methods for measuring P volatility of engine oils were reported –TGA of pure additive – did not give representative results –Modified Noack (PEI) – P losses for some ashless compounds tended to be overstated (see next slides) Bench test conditions for measuring P volatility of engine oils should be similar to actual engine conditions, e.g. –Bulk oil in crankcase (~150C) for hours –Thin oil film on piston ring/liner (~250C) for seconds/minutes

ESCIT 2006 ©Ciba Specialty Chemicals Nitrogen 10 min Tested lubricant Adsorbent (Tenax) Heat shock Step 1)Stripping and adsorption 150°C 2)Desorption and analysis Stripping and adsorption 250°C 3)Desorption and analysis * Gas Chromatograph with, in parallel, a phosphorus detector and a FID (C, H) GC* Tested lubricant Adsorbent (Tenax) Heat shock Nitrogen 10 min GC* New Test Overview : Thin film N 2 stripping thin oil layers Thin film N2 stripping addresses piston ring/liner model

ESCIT 2006 ©Ciba Specialty Chemicals Phosphorus losses from thin oil layers Noack PEI 250 : DTP 1 is known to volatilise in engine Losses are measured as volatilization of phosphorus from formulated oils (0.03 % P in Euro IV oil) over a thin film at 150 and 250 °C for 10 minutes DTP 1 is known to volatilize in engine whereas DTP2 does not ! PEI 250 mot representative

ESCIT 2006 ©Ciba Specialty Chemicals New Test Overview : Phosphorus losses from bulk oil Realistic Exposure and Ageing conditions 160 o C bath Gas inlet -- 5 l/h O 2 Dissolved catalysts ppm Fe ppm Cu Off gas to condensate trap for collection Measure P content IP 48 apparatus Bulk oil aging addresses the crankcase model

ESCIT 2006 ©Ciba Specialty Chemicals DTP 1 is known to volatilize in engine whereas DTP2 does not ! PEI250 mot representative Phosphorus losses from bulk oil Noack PEI 250 :

ESCIT 2006 ©Ciba Specialty Chemicals. Catalyst (TWC) compatibility Tests Results It is clear from this figure that oil B1 causes a much lower increase in emission compared to oil A. Ref: Jens Franz et all, SAE Deactivation of TWC as a Function of Oil Ash Accumulation A Parameter Study Oil A Oil B1 S, ppm P, ppm Ca, ppm Mg, ppm Zn, ppm Calculated For Oil 7500 ppm P (CO)

ESCIT 2006 ©Ciba Specialty Chemicals Waiting for results – correlation? Results PEI 165

ESCIT 2006 ©Ciba Specialty Chemicals Ciba Specialty Chemicals MAKES NO REPRESENTATION OR WARRANTY, EXPRESS OR IMPLIED, INCLUDING OF MERCHANTABILITY OR FITNESS FOR A PARTICULAR PURPOSE. No statements herein are to be construed as inducements to infringe any relevant patent. Under no circumstances shall Ciba Specialty Chemicals be liable for incidental, consequential or indirect damages for alleged negligence, breach of warranty, strict liability, tort or contract arising in connection with the product(s). Buyer’s sole remedy and Ciba Specialty Chemicals’ sole liability for any claims shall be Buyer’s purchase price. Data and results are based on controlled or lab work and must be confirmed by Buyer by testing for its intended conditions of use. The product(s) has not been tested for, and is therefore not recommended for, uses for which prolonged contact with mucous membranes, abraded skin, or blood is intended; or for uses for which implantation within the human body is intended. Summary Ciba is offering an alternative phosphorous volatilization test to the industry Results appear promising and applicable to industry’s stakeholder objectives Seeking industry support to continue evaluation Interested in collaborating with interested parties

ESCIT 2006 ©Ciba Specialty Chemicals