How to Analyze Elemental Impurities in Crude Oil

This article is based on a poster originally authored by Oliver Buettel & Siqi Sun, Ph.D.

Various metals can negatively affect the refining process and the final product's performance. Therefore, they must be examined in crude oil.

However, crude oil may comprise particles, and organic solvents can destabilize plasma.

Organic matrices can cause carbon deposits in the torch and produce signal drift. Therefore, extensive stability is necessary to perform regular analyses.

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Method and Materials

Crude oil specimens are integrated by sonicating at 60 °C for 30 minutes.

Specimens are diluted at 1:20 in Xylene or other standardized solvents. Yttrium internal standard is used.

Calibration: 0.5-10 mg/kg, utilizing organometallic guidelines and blank oil in Xylene.

Table 1. System configuration and set-up of the sample introduction system. Source: Analytik Jena US

Parameter Setting
RF Power 1400 W
Plasma gas flow 15 L/min
Nebulizer gas flow 0.35 L/min
Auxilary gas flow 1.5 L/min
Spray chamber borosilicate cyclonic spray chamber with dip tube, 50 mL
Injector quartz, inner diameter 1 mm
Nebulizer borosilicate concentric nebulizer, 1 mL/min
Outer tube/inner tube quartz/quartz
Pump tubing Viton
Sample pump rate 1 mL/min
Read delay 30 s
Rinse time 45 s

 

Analytik Jena Technology

The V-Shuttle Torch

The V-Shuttle Torch provides a leading vertical arrangement for optimum matrix tolerance with no soot. It is removable and does not require realignment. Consumable costs are minimal, and oxygen can be added.

How to Analyze Elemental Impurities in Crude Oil?

Image Credit: Analytik Jena US

High-Resolution Array ICP-OES

  • Highest resolution: 2 pm @ 200 nm CCD detector for parallel corrections and analyses.
  • Completely automated background correction, including complex spectra.
  • A durable RF generator with exceptional matrix handling and extended stability

Only a few picometers apart, the Cadmium and Arsenic line are well-separated and can be used analytically without difficulty.

Only a few picometers apart, the Cadmium and Arsenic line are well-separated and can be used analytically without difficulty. Image Credit: Analytik Jena US

How to Analyze Elemental Impurities in Crude Oil?

Image Credit: Analytik Jena US

Table 2. Method Detection Limits and crude oil sample results. Source: Analytik Jena US

Element MDL (mg/kg) Crude 1   Crude 2   Crude 3  
Conc. (mg/kg) RSD (%) Conc. (mg/kg) RSD (%) Conc. (mg/kg) RSD (%)
Al 0.05658 2.0718 1.63 2.0028 0.84 1.9251 3.49
Ca 0.06446 4.4366 1.96 2.9558 1.62 3.7576 1.35
Cu 0.01776 0.43911 1.08 0.48229 1.14 0.44543 1.25
Fe 0.01144 20.224 1.35 15.203 0.03 20.119 0.6
Mg 0.00516 0.83873 0.82 0.87692 0.32 0.8875 0.26
Na 0.05522 9.598 1.27 10.057 0.76 7.5746 1.73
Ni 0.01758 38.377 0.97 28.989 0.49 39.934 0.33
P 0.0968 <MDL   <MDL   <MDL  
Si 0.04732 13.285 1.02 8.7253 0.33 13.135 1.24
V 0.0043 28.591 0.43 19.044 0.20 25.192 0.06
Zn 0.0063 2.0102 1.28 2.3580 0.38 0.7139 0.79

 

Figures of Merit

Extended Stability (4 hours):

  • QC Standard: < 10% deviation
  • Specimen replicate analyzes: < 5% RSD.

Method Detection Limit (MDL) < 0.1 mg/kg for all elements (incl. dilution factor).

Spike recovery: 90-110% for all elements

Calibration: R2 >0.998 for all elements

Conclusion

PlasmaQuant PQ9000 has the exceptional ability to analyze trace metals in Crude Oil simple specimen preparation.

Ashing tests are not necessary with an easy to use and maintain system. Robust plasma provides accurate, precise and extended stability with exceptional performance even for difficult specimens.

PlasmaQuant PQ9000 is engineered for excellence.

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This information has been sourced, reviewed and adapted from materials provided by Analytik Jena US.

For more information on this source, please visit Analytik Jena US.

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