Managing the challenges of analyzing battery materials using triple quadrupole inductively coupled plasma mass spectrometry (ICP-MS) equipped with Argon Gas Dilution

Importance of the Topic

Lithium-ion batteries are central to the transition to electric vehicles and energy storage. Monitoring both major components and trace elemental impurities in battery materials is critical for performance, safety, and sustainability. High concentrations of dissolved solids in cathode materials pose analytical challenges that require specialized methods for accurate, rapid, and reliable elemental analysis.

Aims and Study Overview

This work demonstrates a robust analytical approach for determining critical trace impurities in concentrated cathode solutions containing up to 5.3 percent total dissolved solids. The goal is to achieve high sensitivity, accuracy, and throughput by combining triple quadrupole inductively coupled plasma mass spectrometry with argon gas dilution.

Methodology and Instrumentation Used

A Thermo Scientific iCAP TQe ICP-MS equipped with the argon gas dilution option was employed. The sample introduction system included a PFA microflow nebulizer, a baffled cyclonic spray chamber cooled to 2.7 degrees C, a quartz torch with a removable quartz injector, and a peristaltic pump. A humidifier was used to improve sensitivity for high ionization potential elements. Measurements were performed in single quadrupole mode with helium kinetic energy discrimination and in triple quadrupole mode with oxygen reaction gas. The Qtegra software Reaction Finder and autotune routines optimized all analysis conditions.
Sample preparation involved closed vessel microwave and hotplate acid digestions using high purity nitric and hydrochloric acids, followed by filtration and final dilution to approximately 1 percent matrix load. An online internal standard addition ensured correction of matrix effects.

Main Results and Discussion

• Complete microwave digestion and partial hotplate digestion produced consistent nickel to manganese and nickel to cobalt ratios in a cathode standard with an RSD of 1.4 percent.
• He KED mode achieved excellent linearity and low detection limits for most elements but yielded false positives for arsenic and selenium due to polyatomic interferences from nickel oxide and cobalt oxide.
• Triple quadrupole mode with oxygen effectively eliminated these interferences, reducing arsenic from 16.5 to 0.3 milligrams per kilogram and selenium to below 0.04 milligrams per kilogram.
• Method detection limits for fifty one elements were achieved at sub milligram per kilogram levels in solid samples and sub milligram per liter in solution matrices.
• Spike recoveries ranged from 83 to 115 percent and continuing calibration verifications across 202 samples over fourteen hours showed recoveries between 89 and 117 percent with an overall RSD of 5.2 percent.

Benefits and Practical Applications

This method allows direct analysis of high matrix battery materials without time consuming manual dilution, improving throughput and reducing downtime. It supports quality control in battery manufacturing and recycling by providing reliable multi element data including critical impurities.

Future Trends and Applications

Further development may include direct on line monitoring of battery production streams, coupling with automated digestion systems, real time process control, and expansion to new battery chemistries. Integration with data management platforms will facilitate predictive maintenance and sustainability initiatives in battery research and manufacturing.

Conclusion

The combination of argon gas dilution and triple quadrupole ICP-MS offers a powerful solution for the analysis of complex battery cathode materials. This approach achieves low detection limits, robust interference removal, and high throughput, making it well suited for modern laboratories engaged in battery development and recycling.

References

• Thermo Fisher Scientific Brochure 53130 Chemical Elemental and Structural Analysis of Batteries Application Compendium
• Thermo Fisher Scientific Application Note 44463 Robust and Accurate Analysis of Refined Nickel Using Triple Quadrupole ICP-MS
• Thermo Fisher Scientific Application Note 43403 Determination of Elemental Impurities in Vitamin B12 Supplements Using Triple Quadrupole ICP-MS