The Importance of Elemental Analysis for Battery Recycling

The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources The Importance of Elemental Analysis for Battery Recycling 2 The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources The need for lithium ion batteries (LIBs) is rapidly surging due to the soaring demands of efficient renewable energy storage and electric vehicles. However, this raises concerns over the availability of critical raw materials for battery production, many of which are already in limited supply. The LIB recycling process is often complex due to a lack of standardization in battery design and chemistry across the industry. Inductively coupled plasma optical emission spectroscopy (ICP-OES) is a key analytical technique in LIB recycling, allowing accurate, rapid elemental analysis of recycled battery material, to support efficient metal recovery and refinement. Efficient recycling processes are essential for recovering materials for reuse. This eBook explores the applications of ICP-OES in battery recycling and how Agilent solutions are overcoming challenges in the field and ensuring a more efficient and sustainable future for the LIB industry. Foreword 3 The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources Mechanical Separation End of Life Battery Battery Manufacturing Black Mass Cathode, Anode and Metals Separation Battery use Recovery and Upcycling 5 Reasons You Need Onsite Metals Analysis Capabilities for Battery Recycling 4 The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources Mechanical Separation Black Mass Recovery and Upcycling Cathode, Anode and Metals Separation Waste Monitoring Mechanical Separation Black Mass Recovery and Upcycling Cathode, Anode and Metals Separation Waste Monitoring Mechanical Separation Black Mass Recovery and Upcycling Cathode, Anode and Metals Separation Waste Monitoring Mechanical Separation Black Mass Recovery and Upcycling Cathode, Anode and Metals Separation Waste Monitoring Mechanical Separation Black Mass Recovery and Upcycling Cathode, Anode and Metals Separation Waste Monitoring 1 Monitoring airborne particulates Mechanical separation e.g. shredding, creates airborne particulates, hazardous to human health and the environment. ICP-OES can be used to monitor air filters to ensure regulatory compliance. 3 Monitoring and optimizing recycling processes Efficient separation is vital for effective downstream processing. Onsite ICP-OES enables real-time monitoring and optimization at each stage, maximizing material recovery like feedstock chemicals. 2 Analyzing black mass The powder from separation, known as “black mass”, is widely refined through hydrometallurgical and pyrometallurgical processes. ICP-OES effectively measures impurities to ensure the final product quality meets specifications. 4 Ensuring QC of input chemicals Purity of chemicals used in battery recycling is crucial to avoid introducing contaminants in the final product. For example, leaching – a common purification step – uses strong acids and solvents to isolate compounds. 5 Monitoring environmental discharges Thorough chemical analysis of emissions and waste can be achieved using ICP-OES to ensure the correct and safe disposal of these by-products. eBook: A Practical Guide to Elemental Analysis of Lithium Ion Battery Materials Using ICP-OES Battery materials are often difficult to analyze due to dirty sample types and require specific approaches to ensure accurate measurement. Download this ebook to learn tips and tricks overcome common issues faced when analyzing battery materials. DE-003202 This information is subject to change without notice. © Agilent Technologies, Inc. 2024 Published in the USA, December 10, 2024 5994-8002EN 5 The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources The demand for lithium-ion batteries (LIBs) has rapidly surged in recent years due to the increasing adoption of electric vehicles (EVs) and the growing need for efficient renewable energy storage. This is mirrored by the transport sector where EV sales soared from 3 million in 2020 to 17 million in 2024.2 In 2024, global battery storage deployments increased by 53% to 205 gigawatt-hours (GWh), with lithium-ion batteries accounting for 98% of grid-scale installations.1 Optimizing Lithium-Ion Battery Recycling With ICP-OES 6 The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources 1.64 Mt Supply 3.1 Mt Demand However, meeting this increasing demand presents significant challenges. By 2030, battery production is projected to require 3.1 million metric tons of lithium, 3 exacerbating concerns over the scarcity of critical raw materials, many of which are already in limited supply or expected to disappear within decades.4 Cu 29 63.55 Copper Mn 25 54.94 Manganese Li 3 6.94 Lithium Ni 28 58.69 Nickel Si 14 28.08 Silicon C 6 12.01 Carbon Al 13 26.98 Aluminum Co 27 58.93 Cobalt 7 The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources Currently, only 5% of discarded LIBs are recycled globally.5 This is partially due to the recycling process complexity and high cost. Since battery design and chemistry aren’t standardized throughout the industry, batteries differ significantly between manufacturers. Each battery type may require tailored methods for disassembly, material extraction and purification. Consequently, thorough material screening is essential for process efficiency and to ensure the purity of recovered materials. In this infographic, we will explore the process of battery recycling, highlight the role of advanced analytical techniques and discover innovations shaping the future of sustainable LIB recycling. Decrease reliance on mining Reduce environmental impact Alleviate resource limitations Recycling and recovery of secondary raw materials from spent batteries can help 8 The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources HYDRO PROCESS RECYCLING Lithium-Ion Battery Recycling Battery use Landfill Second use Battery manufacturing Refining Cathode production Mining PYRO PROCESS RECYCLING DIRECT RECYCLING How are LIBs recycled? Current commercial recycling technologies for LIBs primarily rely on pyrometallurgical and hydrometallurgical methods.6 These technologies generate recovered materials at different stages of the recycling process, which can then be refined and repurposed for new battery production. Pyrometallurgical recycling involves smelting entire batteries or pretreated components, producing a metallic alloy, slag and gases. The metal alloy is further processed using hydrometallurgical techniques to separate individual metals. Hydrometallurgical recycling involves solvent leaching and subsequent recovery of battery materials through methods such as solvent extraction and precipitation. Direct recycling restores used battery materials without breaking them down completely. This method has the potential to offer significant economic and environmental benefits but is still in the early stages of development.7 9 The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources What role does analytical characterization play in LIB recycling? All LIB recycling processes require analytical characterization to determine elemental composition, purity and contamination levels. 40% 25% 10% 5% 5% 15% First, used LIBs are shredded or crushed to produce black mass. Black mass contains a mixture of valuable metals essential for manufacturing new batteries. Graphite Other (including Al, Cu, Fe) Lithium Manganese Nickel Cobalt % are indicative of NMC battery chemistry Accurate chemical analysis methods are essential for analyzing the elemental composition of black mass, enabling efficient extraction and refinement. Techniques like inductively coupled plasma optical emission spectroscopy (ICP-OES), X-ray fluorescence (XRF), scanning electron microscopy (SEM) and atomic absorption spectroscopy (AAS) are widely used for this purpose. In later stages, during the separation and purification of black mass into battery-grade feedstock materials, elemental analysis also ensures both the efficiency of the process and the purity of the final materials. 10 The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources Why is ICP-OES essential to optimize LIB recycling? ICP-OES is a key analytical technique in battery recycling, providing rapid and precise multi-element analysis. The black mass is first dissolved into a liquid solution, then atomized and ionized using high-temperature plasma. ICP-OES measures the wavelengths emitted from this sample, enabling accurate identification and quantification of key elements. ICP-OES is more sensitive than XRF and AAS and is used when speed and precision are required, particularly for the detection of trace elements. From analyzing black mass composition to ensuring the purity of battery-grade materials, ICP-OES enables scalability in industrial recycling operations. The key advantages of ICP-OES include: Multi-element analysis Simultaneously detects and quantifies over 70 elements, including lithium, nickel and cobalt. Wide dynamic range Efficiently measures both high-concentration elements and trace impurities, ensuring comprehensive material characterization. ICP-OES Efficiency High throughput and streamlined workflows make it well-suited for large-scale recycling operations. High sensitivity and precision Provides accurate results essential for assessing black mass value and optimizing recovery processes. Matrix tolerance Effectively handles the complex and heterogeneous nature of black mass samples with minimal interference, maintaining data reliability. 11 The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources The future of LIB recycling The global volume of LIB waste is projected to reach approximately 11 million tons by 2030.8 To address this challenge, advanced recycling technologies are emerging to improve material recovery, reduce waste and minimize the environmental impact of the recycling process: Direct upcycling Recycled materials can be used to create better-performing battery components, a process that is more flexible than direct recycling but still requires further development.9 Emerging techniques Innovations like bioleaching (using bacteria to extract metals), supercritical CO2 (a highpressure, high-temperature solvent) and electrochemical methods are promising techniques that could further reduce costs and environmental harm.10, 11, 12 Smart elemental analysis tools The Agilent 5800 ICP-OES integrates intelligent software to simplify method development and minimize spectral interference. During analysis, it also automatically detects and flags any nebulizer issues. 12 The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources Towards a sustainable future As the demand for LIBs rises, efficient recycling is essential for recovering high-purity materials for reuse. Innovative recycling technologies and advanced elemental analysis, like ICP-OES, are key for optimizing material recovery, reducing waste and ensuring smoother operations. With smarter analytical tools, LIB recycling can be faster, cleaner and more reliable, paving the way for a greener, more sustainable energy future. Discover how ICP-OES can streamline your battery recycling workflow. References: 1. Murray, C. Global BESS deployments soared 53% in 2024. Energy-Storage News. https://www.energy-storage. news/global-bess-deployments-soared-53-in-2024/ 2. Over 17 million EVs sold in 2024 - Record Year. Rho Motion. https://rhomotion.com/news/over-17-million-evssold-in-2024-record-year/ (accessed 2025-02-13). 3. Global lithium supply & demand 2022-2030. Statista. https://www.statista.com/statistics/1421980/globallithium-supply-and-demand/ (accessed 2025-02-13). 4. Xu, C.; Dai, Q.; Gaines, L.; Hu, M.; Tukker, A.; Steubing, B. Future Material Demand for Automotive LithiumBased Batteries. Commun Mater 2020, 1 (1), 1–10. https://doi.org/10.1038/s43246-020-00095-x. 5. Etude, M. C.; Ikeuba, A. I.; Njoku, C. N.; Yakubu, E.; Uzoma, H. C.; Mgbemere, C. E.; Udunwa, D. I. Recycling Lithium-Ion Batteries: A Review of Current Status and Future Directions. Sustain Chem 2024, 4, 100027. https://doi.org/10.1016/j.scowo.2024.100027. 6. Gaines, L. Lithium-Ion Battery Recycling Processes: Research towards a Sustainable Course. SM&T 2018, 17, e00068. https://doi.org/10.1016/j.susmat.2018.e00068. 7. Harper, G.; Sommerville, R.; Kendrick, E.; Driscoll, L.; Slater, P.; et al. Recycling Lithium-Ion Batteries from Electric Vehicles. Nature 2019, 575 (7781), 75–86. https://doi.org/10.1038/s41586-019-1682-5. 8. Lv, H.; Huang, H.; Huang, C.; Gao, Q.; Yang, Z.; Zhang, W. Electric Field Driven De-Lithiation: A Strategy towards Comprehensive and Efficient Recycling of Electrode Materials from Spent Lithium Ion Batteries. App Catal B: Environ 2021, 283, 119634. https://doi.org/10.1016/j.apcatb.2020.119634. 9. Ma, X.; Meng, Z.; Bellonia, M. V.; Spangenberger, J.; Harper, G.; Gratz, E.; et al. The Evolution of Lithium-Ion Battery Recycling. Nat. Rev. Clean Technol. 2025, 1 (1), 75–94. https://doi.org/10.1038/s44359-024-00010-4. 10.Moazzam, P.; Boroumand, Y.; Rabiei, P.; Baghbaderani, S. S.; Mokarian, P.; Mohagheghian, F.; et al. Lithium Bioleaching: An Emerging Approach for the Recovery of Li from Spent Lithium Ion Batteries. Chemosphere 2021, 277, 130196. https://doi.org/10.1016/j.chemosphere.2021.130196. 11.Cattaneo, P.; D’Aprile, F.; Kapelyushko, V.; Mustarelli, P.; Quartarone, E. Supercritical CO2 Technology for the Treatment of End-of-Life Lithium-Ion Batteries. RSC Sustain. 2024, 2 (6), 1692–1707. https://doi.org/10.1039/ D4SU00044G. 12.Kityk, A.; Pavlik, V.; Hnatko, M. Reshaping the Future of Battery Waste: Deep Eutectic Solvents in Li-Ion Battery Recycling. J. Energy Storage 2024, 97, 112990. https://doi.org/10.1016/j.est.2024.112990. 13 The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources Towards the Future of Battery Recycling Approximately 95% of lithium-ion battery (LIBs) components can be recycled, to be used in new batteries or other industries. LIB recycling holds a wide range of advantages – including maintaining stable supply chains, environmental protection and cost efficiency. Due to the variable chemistry of LIBs, elemental analysis techniques are essential in identifying and quantifying the elemental composition of recycled batteries. Inductively coupled plasma optical emission spectroscopy (ICP-OES) is one such method of analysis, and is used to: However, battery recycling can pose challenges that affect the efficiency and effectiveness of ICP-OES analysis. Here, we explore these challenges and examine how cutting-edge software and instrumentation can improve workflow efficiency. Measure the elemental content of black mass to give guidance on metal salt recovery and method optimization for maximum yield Determine the purity of recycled battery materials Monitor environmental discharge and worker safety 3 Li Mn Co Ni 25 27 28 14 The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources The challenges of ICP-OES-based analysis The black mass made from shredded post-consumer batteries can pose multiple challenges to ICP-OES-based analysis and quantification. High amounts of dissolved solids Wide range of elemental concentrations High concentrations of lithium ions can affect the measurement of trace elements e.g., Na and K High background signals and interference Lithium can degrade instrument components 15 The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources How does the Agilent ICP-OES do it better? The 5800 and 5900 Agilent ICP-OES have a range of embedded features, including innovative software, that can improve throughput and streamline workflows. These features give time back to lab operators and offer unparalleled insights into samples. The smart systems provide alerts to problems before they occur, maximizing efficiency, increasing accuracy and minimizing sample re-measurement 1 IntelliQuant Screening elemental “heat map” showing which elements are present in a black mass sample, and the semi-quantitative concentration (ppm) Simplifies method development When analyzing black mass, the unknown concentration of elements can make selecting a calibration range difficult. As a consequence, re-measurement of samples that fall outside the calibration are common. The Agilent ICP Expert Pro Software features the IntelliQuant Screening smart tool which helps to simplify method development. IntelliQuant Screening runs a rapid scan that semi-quantitates the concentrations of elements present in unknown samples. This can then be used to generate an optimum calibration concentration range for the full quantitative scan, reducing the chance of sample re-measurement. Results are generated in a simple, intuitive “heat map” format for easy identification. In addition, IntelliQuant generates automated spectral interference identification and suggests the best wavelength to use to avoid interference. IntelliQuant Screening elemental “heat map” showing which elements are present in a black mass sample, and the semi-quantitative concentration (ppm) 16 The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources 2 3 Automatically dilutes samples The Agilent Advanced Dilution System (ADS 2) is designed specifically for Agilent instruments to enable rapid measurements of multiple major and trace elements in lithium salts. Autodilution systems minimize the risk of routine errors during sample preparation, especially for less experienced operators, while significantly reducing sample preparation time and helps to ensure the right result the first time, improving analysis efficiency. Features of the ADS 2 include: Increases rinse efficiency In facilities handling large numbers of samples, efficiency is key to reduce both time and reagent consumption. The Intelligent Rinse function within the Agilent ICP Expert Pro Software controls the time required to rinse the sample introduction after each sample, depending on the intensities of nominated element signals. The software automatically ends the rinse when the element intensities reach a userspecified threshold, meaning that both sample throughput and argon consumption are optimized. AUTOCALIBRATION Fully automated calibration from a single stock solution PRESCRIPTIVE DILUTION Automatic dilution of samples by a known dilution factor SUMMARY ROW Selects the best result from available measurements reducing data processing REACTIVE DILUTIONS Automated dilutions in response to over-range samples 17 The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources Automatic background correction Battery material samples can contain a wide range of elements of varying concentrations. This can lead to high levels of complex background signals, making background correction and the placement of background markers difficult, affecting the accuracy of results. 4 Difficulty placing background markers In complex samples, emission peaks for elements of interest can be surrounded by high background peaks, making manual peak identification difficult and leading to inaccurate results. SOLUTION The Agilent fitted background correction (FBC) technique uses an algorithm to automatically correct for background, removing guesswork and improving accuracy and detection limits. High background signals High background signals must be corrected for. If the background correction is inaccurate, the baseline will slope, resulting in an incorrect result. SOLUTION The Agilent fitted background correction (FBC) technique can be used to automatically correct for the effects of a sloping baseline, improving detection limits and reducing overcorrection. 18 The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources Prevents nebulizer blockages Battery black mass analysis can impact sample introduction systems. Lithium can damage plasma torches, and hydrofluoric acid used to digest samples can also digest glass components. In addition, organic chemicals can cause pump tubing to degrade, resulting in reduced precision and measurement drift. This can be solved using a range of strategies to increase component life and reduce costs: 5 Instead of a one-piece torch, a fully demountable torch allows the operator to replace just the worn components, instead of the whole torch Inert sample introduction kits made from hydrofluoric acid-resistant materials ensure long-lasting performance Agilent’s solvent resistant tubing Solvaflex can withstand the organic chemicals in battery analysis A switching valve can reduce the exposure time that instrument components are in contact with damaging materials Get the edge over the competition with Agilent Battery material analysis is complex and can give rise to numerous challenges. However, Agilent ICP-OES and consumables can overcome these challenges and help you achieve unparalleled accuracy and efficiency. Discover how you can get the right result the first time. Learn more about the Agilent ICP-OES range 19 The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources Application Compendium Recovery of Metals in Green Solvents by ICP-OES Read this application note to discover how to use ICP-OES to analyze elements of spent LIBs in biodegradable deep eutectic solvents. Elemental Analysis of Lithium-Ion Battery Black Mass Recycling Material by ICP-OES Read this application note to learn how ICPOES is used to support the recovery of valuable metals from spent lithium-ion batteries. Analysis of Waste Samples According to the US EPA Method 6010D Read this application note to learn how Agilent ICP-OES instruments can help simplify method development and meet regulatory guidance. Enhanced RoHS Compliance Testing with Agilent 5800 ICP-OES Read this application note to learn how ICP-OES can accurately monitor the levels of multiple hazardous elements in plastics. Workplace Air Monitoring: MultiElement Analysis of Air-Filters using ICP-OES Read this application note to explore how ICP-OES can rapidly analyze 44 elements to ensure healthy workplace air quality. Click here Click here Click here Click here Click here 20 The Importance of Elemental Analysis for Battery Recycling Metals analysis capabilities Optimizing recycling Advancing workflows Resources Determination of Metals in Recycled Liion Battery Samples by ICP-OES Read this application note to learn how to quantify 18 different metals in black mass. Elemental Analysis of Intermediate Feedstock Chemicals for Li-Ion Batteries (LIBs) by ICP-OES Read this application note to discover methods for quality control of unrefined cathode-metal solutions from LIBs. The Fastest and Smartest Way to Analyze Water Samples by ICP-OES Read this application note to explore how ICP-OES can enable fast and reliable regulation-compliant water analysis. Determination of Multiple Elements in Lithium Salts using Autodilution with ICP-OES Read this application note to learn how to reduce waste and avoid human-induced error with automated analysis of LIB precursor chemicals. Reducing Instrument Downtime in Elemental Analysis of Lubricant Oils as per ASTM 5185 Read this application note to explore methods for faster and longer sample suns with the V-grove nebulizer. Click here Click here Click here Click here Click here