Degradation of lithium ion (Li-ion) cells affects both performance and safety of Li-ion batteries. In order to avoid potential safety hazards, it is crucial to detect the onset and extent of critical degradation modes in commercial Li-ion cells. This work demonstrates the application of a diagnostic algorithm to identify and quantify degradation modes of commercial Li-ion pouch cells cycled at −10 • C and a C-rate of 2 C. Rapid loss of active negative electrode material was successfully identified and results were validated using 3-electrode cells, scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). The positive electrode material was less strongly affected by the tests, as found by the diagnostic algorithm and confirmed with EDX and SEM results. Lithium ion (Li-ion) cells degrade as a result of usage and environmental influences, typically resulting in capacity fade and increased internal resistance.1-3 Some degradation mechanisms can lead to safety hazards through increased risk of fire or explosion. The deposition of metallic lithium and dendrite formation on graphite negative electrodes (NE) are particularly dangerous mechanisms, since metallic dendrites can pierce the separator and lead to internal short-circuits resulting in thermal runaway. [4][5][6] Understanding and detecting lithium plating and dendrite formation are important milestones on the pathway to safer, more reliable Li-ion batteries. Low operating temperatures during charge increase the risk of lithium plating and dendrite formation. [7][8][9][10][11][12][13][14][15][16] This makes it important to assess and model the behavior of Li-ion batteries at low temperatures, which is undertaken in this study.Arora et al. 4 proposed a mathematical model to predict lithium deposition on the NE during charge and overcharge, which can be used to determine operational and design limitations in order to minimize safety hazards. Other authors have focused on in-situ detection of lithium plating using electrochemical calorimetry, 17 a combination of an electrochemical model with a particle filter, 18 Although in-situ detection of lithium plating is an important advance, safety hazards can be further reduced by detecting the factors leading up to lithium plating before the onset of the plating mechanism itself. Deposition of metallic lithium on graphite NEs occurs under high charging rates, at low charging temperatures and in poorly balanced cells with an excess of active positive electrode (PE) material. 4,12,24,25 These circumstances are easily avoided in new cells by appropriate cell design and observation of operational limitations such as minimal charging temperature and maximal cell voltages and current rates. However, as cells degrade, active electrode material can be lost, changing the ratio of negative to positive electrode material and the current rates and voltage limits imposed on the remaining active material. Loss of NE material leads to higher current rates on the NE and a higher ratio of active PE to NE material...