Analysis of Wear Metals in Lubricating Oil ICP-OES & ASTM Methodology Advanced Research Center 106 Access Rd, Suite 3 Norwood, MA Slide info courtesy of SPECTRO Analytical Instruments 91 McKee Dr Mahwah NJ 07430

2 Main petrochemical applications  Blending control of fresh lubricants, greases and control of the additive packages  Used oil analysis  Analysis of sulfur content in crude oil distillates  Analysis of sulfur and trace element content in crude oil and residual heavy fuel  Analysis of trace element content in diesel/biodiesel fuel

3 What is a lubricating oil  Lubricating oils are formulated with a number of chemicals blended into base oils to provide products that  last longer  keep machinery cleaner  allow the machinery to work better under severe operating conditions  These organic chemicals, better known as additives, contain organometallic and inorganic compounds as their active ingredients  Lubricating oils contain: – % base oil – % additive package – % viscosity index improvers (macromolecular compounds with a molecular weight between )

4 Additive packages Elemental range:  B: up to6%  Mg: up to9%  Si: up to13%  P: up to11%  S: up to45%  Cl:up to35%  Ca:up to17%  K: up to8%  Zn:up to12%  Mo: up to 8.5%

5 Type of lubricating oils  Engine oils – Ca between ppm – Zn/P between ppm – Mo between ppm – Mg between ppm  Marine oils – Ca between ppm – Zn/P between ppm  Industrial oils – All additives lower than 500 ppm  Transmission oils – Variable

6 Used oil analysis  Determination of additive element content – information pertaining to additive depletion in service and possible charging of the system with the wrong oil – ICP-OES analysis according to ASTM D4951 (9 elements)  Determination of wear element content – information pertaining to increased wear rate and possible abnormal operating conditions – ICP-OES analysis according to ASTM D5185 (22 elements)

7 Wear elements: spectroscopic operating baseline For interpretation of the results trend analysis is more important than an individual reading

8 Condition monitoring elements and their significance

9 Elemental scope for fresh and used lubricants Scope ICP-OES  B, Na, Mg, Si, P, S, Cl, K, Ca, V, Cr, Mn, Fe, Ni, Cu, Zn, Mo, Cd, Sn, Sb, Ba, Pb Scope XRF  B, Na, Mg, Si, P, S, Cl, K, Ca, V, Cr, Mn, Fe, Ni, Cu, Zn, Mo, Cd, Sn, Sb, Ba, Pb  Note: B, Na, and Mg are not as analytically accurate by XRF!

10 PARTICLE COUNTING: Relation between particle size and percentage of recover

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