Elemental Analysis of Lithium-Ion Battery Black Mass Recycling Material by ICP-OES

Importance of the Topic

As the volume of spent lithium-ion batteries grows, recovering valuable metals from black mass (BM) reduces environmental impact, decreases reliance on primary mining, and minimizes toxic waste. Robust, accurate elemental analysis of BM is essential for determining material value and ensuring safe recycling processes.

Objectives and Study Overview

This study evaluates the performance of the Agilent 5900 SVDV ICP-OES equipped with an inert V-groove nebulizer for direct, unfiltered analysis of acid-digested BM samples. Key goals include assessing accuracy, precision, long-term stability, and reduced sample preparation requirements.

Methodology and Instrumentation

• Sample Preparation: BM powder acid-digested in aqua regia, diluted without filtration or settling.
• Instrumentation: Agilent 5900 SVDV ICP-OES with high-TDS inert V-groove nebulizer, inert cyclonic double-pass spray chamber, Easy-fit torch with 2.4 mm alumina injector, and SPS 4 autosampler.
• Calibration and Background Correction: Multi-element calibration standards in 10% HNO3, FACT spectral deconvolution applied to Na 589.592 nm line to correct Ba interference, and carefully chosen wavelengths to minimize spectral overlaps.
• Operating Conditions: RF power 1.40 kW, plasma gas 15 L/min, nebulizer gas 0.90 L/min, read time 5 s, three replicates per sample.

Main Results and Discussion

• Quantified 20 elements in BM with mean RSDs below 7.8%, covering mg/kg to percent levels.
• Spike recovery tests showed recoveries within ±10% for all analytes at low and high concentrations.
• Analysis of unfiltered, settled, and filtered aliquots differed by less than 5%, demonstrating that filtration or settling is unnecessary.
• Method detection limits ranged from 0.02 to 3.5 mg/kg across elements.
• In a 16-hour continuous run with QC checks every 15 samples, concentrations remained within ±10% of initial values and precision stayed better than 5% RSD. The nebulizer operated blockage-free for over three weeks.

Benefits and Practical Applications

• Eliminates time-consuming filtration and settling steps, reducing consumable use and contamination risk.
• Increases laboratory throughput and minimizes instrument downtime and maintenance costs.
• Provides reliable quality control for battery recycling facilities, supporting efficient recovery of lithium, nickel, cobalt, manganese, and other critical metals.

Future Trends and Possibilities

• Wider adoption of robust nebulizer technology for challenging matrices in e-waste, mining, and environmental analysis.
• Integration with automated high-throughput workflows and real-time data analytics for process optimization.
• Advancement of background correction and spectral deconvolution methods to enhance trace-level detection capabilities.
• Contribution to circular economy initiatives by improving resource recovery and reducing waste generation.

Conclusion

The Agilent 5900 SVDV ICP-OES coupled with an inert V-groove nebulizer delivers precise, stable, and maintenance-friendly multi-element analysis of unfiltered BM digests. This robust approach streamlines laboratory workflows and supports sustainable battery recycling operations.

References

• Li S Determination of Metals in Recycled Li-Ion Battery Samples by ICP-OES Agilent Technologies application note 5994-5561EN 2023
• Real-time Spectral Correction of Complex Samples Using FACT Spectral Deconvolution Software Agilent Technologies technical overview 5991-4837EN 2021