Determination of Essential Metals and Trace Elements in Black Mass using ICPE-9820

Significance of the Topic

The rapid growth of lithium-ion battery use in consumer electronics and electric vehicles has increased demand for critical metals while generating substantial end-of-life waste.
Analyzing black mass, the mixed powder from spent batteries containing valuable metals and impurities, is essential for optimizing recycling processes and reducing environmental impact.

Objectives and Study Overview

This study demonstrates the application of the Shimadzu ICPE-9820 for simultaneous determination of essential metals (Li, Co, Ni, etc.) and trace elements in black mass samples from battery recycling.
Key goals include achieving accurate quantitation across a wide concentration range and minimizing operational costs through reduced argon consumption.

Methodology

A finely ground black mass sample underwent microwave digestion with a mixture of hydrochloric and nitric acids, followed by dilution and filtration to remove residual graphite.
Calibration standards covering trace to major element ranges were prepared from single-element solutions, acid-matched to samples, with yttrium added as an internal standard.

Instrumentation Used

Instrument: Shimadzu ICPE-9820 simultaneous ICP atomic emission spectrometer
Key Conditions:

• RF power: 1.2 kW
• Plasma gas flow: 10 L/min; Auxiliary: 0.6 L/min; Carrier: 0.7 L/min
• Nebulizer: Type 10; Spray chamber: cyclone
• Mini torch; Axial and radial viewing modes

Main Results and Discussion

Calibration curves for all elements exhibited excellent linearity (R>0.9999 for most), with instrument detection limits in the microgram-per-liter range.
Quantitative analysis of two sample replicates revealed high concentrations (>1 wt%) of Al, Co, Cu, Li, Mn, and Ni, with other elements in the mg/kg range.
Spike recovery tests showed recoveries between 93% and 112%, indicating minimal matrix interference and high method accuracy.

Benefits and Practical Applications

The ICPE-9820 enables simultaneous multi-element analysis across a broad concentration spectrum, reducing analysis time and argon gas consumption.
High sensitivity and dual viewing modes support precise quantitation in complex matrices, facilitating process control in battery recycling operations.

Future Trends and Potential Applications

Integration of real-time monitoring and automation could further streamline black mass analysis.
Advancements in plasma technology and data processing may lower detection limits and enhance throughput.
Extending this approach to other electronic waste streams and coupling with speciation techniques could broaden the scope of sustainable recycling analytics.

Conclusion

The Shimadzu ICPE-9820 demonstrates robust performance for comprehensive analysis of essential and trace elements in black mass, offering an efficient, accurate, and cost-effective solution for supporting lithium-ion battery recycling initiatives.

References

1. Kim T., Song W., Son D.-Y., Ono L.K., Qi Y. (2019) Lithium-ion batteries: outlook on present, future, and hybridized technologies. J. Mater. Chem. A 7:2942–2964.
2. Directive 2006/66/EC of the European Parliament and Council (2006) on batteries and accumulators and waste batteries, Official Journal L 266:1–14.
3. Nóbrega J.A., Carnaroglio D., Volpi M., Rota G. (2023) Tackling sample preparation for elemental analysis in the lithium-ion battery industry. Milestone Srl.