ICP-OES Analysis of Copper Recovered from Li-Ion Batteries for Foil Manufacturing

Importance of the Topic

The recycling of lithium-ion batteries (LIBs) and the recovery of copper for foil manufacturing are critical to reducing environmental impact, lowering production costs, and securing supply of key materials. Effective analytical methods are needed to ensure quality control across each stage of battery remanufacturing.

Objectives and Study Overview

This study demonstrates an integrated approach using the Agilent 5800 VDV ICP-OES with automated sample handling to quantify 23 elements in real copper sulfate electrolyte samples recovered from LIB recycling. The aim is to validate method accuracy, precision, and throughput improvements in high-matrix conditions.

Instrumentation

Agilent 5800 VDV ICP-OES equipped with AVS 7 switching valve, ADS 2 autodilutor, SPS 4 autosampler, SeaSpray nebulizer, double-pass cyclonic spray chamber, argon humidifier accessory, and semi-demountable VDV torch. Analysis controlled by Agilent ICP Expert Pro software.

Methodology

Samples of copper sulfate electrolyte in 3 % H₂SO₄ were analyzed without manual preparation. Internal standards (Sc and Rb) compensated for matrix effects. Both axial and radial plasma views were optimized for RF power, nebulizer flow, and viewing height. IntelliQuant Screening guided selection of calibration ranges and emission lines. Calibration standards were prepared automatically by ADS 2 from single- and multi-element stock solutions. Quality control employed a continuing calibration blank and verification standards, with prescriptive and reactive dilutions to keep analytes within range.

Results and Discussion

Calibration curves for all 23 elements exhibited excellent linearity (R² ≥ 0.99999). Method detection limits were in the sub-ppb to low-ppb range even in a high-copper matrix. Spike recovery tests yielded 96–105 % recovery for all elements. A 5-hour stability test of 187 samples demonstrated precision with RSD < 1.3 % and stable nebulizer performance.

Benefits and Practical Applications

Automated dilution and sample handling reduce manual errors and increase throughput. The robust ICP-OES system effectively handles corrosive, high-TDS matrices, providing reliable quality control for LIB recycling streams and copper foil remanufacturing.

Future Trends and Applications

Further integration with advanced software and AI-driven optimization is expected to enhance method development. Expansion to other battery chemistries, real-time process monitoring, and greener analytical protocols will support circular economy goals.

Conclusion

The Agilent ICP-OES Automation System offers a robust, accurate, and efficient solution for multi-element analysis in recovered copper electrolytes. It streamlines workflows, ensures data quality, and supports sustainable battery manufacturing.

References

• Harper G., Sommerville R., Kendrick E. et al. Recycling lithium-ion batteries from electric vehicles. Nature 575, 75–86 (2019).
• Lu L., Liu H., Wang Z. Advances in electrolytic copper foils: fabrication, microstructure, and mechanical properties. Rare Metals 44, 757–792 (2025).
• Agilent. A Practical Guide to Elemental Analysis of Lithium-Ion Battery Materials Using ICP-OES. Agilent Technologies publication 5994-5489EN.
• Agilent. ICP-OES Quality Control of Elements in Brines Produced by Direct Lithium Extraction (DLE). Agilent Technologies publication 5994-8041EN.
• Agilent. Innovative Freeform Optical Design Improves ICP-OES Speed and Analytical Performance. Agilent Technologies publication 5994-5891EN.
• Agilent. Agilent ICP Expert Software: Powerful software with smart tools for ICP-OES. Agilent Technologies publication 5994-1517EN.
• Agilent. ICP-OES Automation Systems. Agilent Technologies brochure.
• Agilent. Capabilities and Operation of the Advanced Dilution System 2. Agilent Technologies publication 5994-7211EN.
• Agilent. Agilent IntelliQuant Screening: Smarter and quicker semiquantitative ICP-OES analysis. Agilent Technologies publication 5994-1518EN.