Laboratory Analyst Training Curriculum
Mod 7 - Metals
Module from the Laboratory Analyst Training Curriculum curriculum.
Module 7 — Metals and Contaminants · Learning Objectives · 1. Apply ICP-OES (D5185) and XRF methods for trace metals in oils. · 2. Measure vanadium and nickel in crude/resid for FCC catalyst impact assessment. · 3. Detect sodium, potassium, and calcium contaminants affecting fired heaters. · 4. Monitor silicon (antifoam) and phosphorus in used oils and fuels. · 5. Control sample prep, dilution, and internal standard techniques. · Metals Methods
| Method | Technique | Scope |
|---|---|---|
| ASTM D5185 | ICP-AES (OES) | Used / new oils, 22 elements |
| ASTM D5708 | ICP / GFAAS | Ni, V in crude and resid |
| ASTM D3605 | AAS | Trace V, Ni in gas turbine fuels |
| ASTM D7691 | ICP-MS | Ultra-trace metals |
| ASTM D4951 | ICP-AES for Lube Additives | P, Zn, Ca, Mg additives |
| ASTM D6595 | RDE-OES | On-site used oil, rotating disk |
| ASTM D5863 | ICP / AAS for Nickel/Vanadium | Residual fuel, crude |
| ASTM D7111 | ICP-AES | Middle distillate trace metals |
| Key Metals — Impact and Limits | ||
| Metal | Source | Impact |
| Vanadium | Crude | FCC E-cat poison; turbine corrosion |
| Nickel | Crude | FCC dehydrogenation; H2/coke |
| Iron | Corrosion | Catalyst poison, coker foam |
| Sodium | Desalter | Fired heater deposits |
| Silicon | Antifoam carryover | Catalyst poison for HDT/HDN |
| Calcium | Naphthenate salts | Crude desalter loading |
| Phosphorus | Additives / pipeline | Catalyst poison |
| Arsenic | Crude contamination | Reformer catalyst poison |
| Lead | Legacy additive | Reformer poison |
| Mercury | Condensates | HSE, equipment corrosion |
| D5185 ICP-OES — Operating Conditions | ||
| Parameter | Typical Value | |
| RF power | 1300–1500 W | |
| Plasma gas (Ar) | 12–17 L/min | |
| Auxiliary gas | 0.5–1.5 L/min | |
| Nebulizer gas | 0.6–0.9 L/min | |
| Dilution solvent | Mixed xylenes or kerosene | |
| Internal standard | Yttrium or cobalt | |
| Calibration | 5-point + blank, org-matrix stds | |
| Sample Preparation | ||
| Matrix | Dilution | Internal Std |
| Used engine oil | 1:10 in xylene | Co at 5 ppm |
| Crude oil | 1:5 in kerosene | Y at 2 ppm |
| Resid | Microwave digest or direct dilute | Y at 2 ppm |
| Fuel oil | 1:5 in mixed xylene | Y or Sc |
| Reformer feed (As) | Hydride generation AAS | — |
| Precision (D5185 Representative) | ||
| Element | Level | r |
| Fe | 50 ppm | 4.0 ppm |
| Cu | 20 ppm | 1.8 ppm |
| V | 10 ppm | 1.1 ppm |
| Ni | 10 ppm | 1.2 ppm |
| Si | 10 ppm | 1.5 ppm |
| Na | 20 ppm | 3.0 ppm |
| ◄ Return to Instructions |
Source: Laboratory_Analyst_Training_Curriculum_v1.xlsx · Sheet: Mod 7 - Metals
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