Establishing an independent and sustainable battery value chain necessitates a closed-loop recycling approach. Recycling end-of-life lithium-ion battery (LIB) cells is critical to prevent their disposal in landfills, where they may release harmful substances into the environment, including fluorine (F), nickel (Ni), manganese (Mn), cobalt (Co), and organic components such as electrolytes and their degradation products. Furthermore, it is crucial to understand the composition of LIB recycling material, referred to as black mass, because these contaminants can undermine business infrastructure, impede recycling efforts, and pose health threats to workers.
This study developed a workflow for measuring electrolyte residues, including both linear and cyclic carbonates, conducting salts, and selected degradation products from shredded lithium-ion battery black mass. A LC-MS/MS technique was established to separate and accurately quantify standard organic electrolyte compounds with low detection and quantification limits. For measuring ionic species, IC-CD was employed. It was observed that up to 5.5 wt.% of organic compounds and 2.8 wt% of ionic species could be extracted from the black mass. The most prevalent compounds identified were ethylene carbonate and hexafluorophosphate. The use of protic solvents such as water and methanol led to the formation of ethylene glycol and fluoride through degradation reactions. Additionally, three different extraction methods were assessed, with shake extraction proving to be the most efficient technique for quantitative analysis.