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Lithium-ion batteries are usually installed in portable electronic devices and electric vehicles (EV). Because they are both powerful and lightweight, and their high energy density, they are a popular choice. Lithium ions are present in the positive and negative materials of lithium-ion batteries.
Common daily battery types use lithium graphite (LiC6) as the anode and lithium cobalt oxide (LiCoO2) as the cathode. The manufacture of the cathode material usually includes a calcination step. Combine, mix and heat the solid precursor salts. To produce lithium cobalt oxide (LiCoO2), lithium carbonate (Li2CO3) is mixed with cobalt oxide (Co3O4). This combination is heated in an oxygen atmosphere to produce an active LiCoO2 electrode.
However, chloride salts such as lithium chloride (LiCl) can be found in the final product, which means it is usually not pure. These impurities are considered to be inert in the electrochemical reactions of lithium ion batteries. Therefore, check the chloride content of the cathode material after production.
This experiment outlines a method for determining the chloride content of lithium cobalt oxide-based cathode materials. Initially, nitric acid was used to leaching the powder to dissolve the sample. Subsequently, an aqueous silver nitrate solution was used to titrate chloride ions. Due to the low chloride content, the sample was titrated against the sodium chloride blank solution. The technology is based on the Chinese standard: GB/T 11064.10 2013.
Add 10 mL of nitric acid solution and 30 mL of deionized water to the titration beaker. Start method M830A. The titrator uses a burette to accurately add 10 mL of sodium chloride blank solution, and then titrate with silver nitrate solution.
Expenses in mmol are usually saved as a blank value: B[NaCl].
Mix 2g of LiCoO2 cathode powder and 5 mL of nitric acid solution and add them to a 100 mL glass titration beaker. Stir until the sample is completely dissolved. Then, pour 30 mL of deionized water to rinse the residue into the solution. Place the beaker on the manual titration stand and start the M830B method.
First, the titrator uses a burette to precisely add 10 mL of a blank solution of sodium chloride, and then uses a silver nitrate solution for titration. Subtract the blank value B[NaCl] from the original result to get the chloride content in the sample.
Image source: METTLER TOLEDO-Titration
Cl- + AgNO3 → AgCl + NO3 –
Titrant: Aq. Silver nitrate solution, AgNO3, c = 0.005 mol/L. Blank solution: Aq. Sodium chloride solution, NaCl, c = 0.2 g/L. Sample: lithium cobalt oxide cathode material. Analytes: chloride, Cl-, M(Cl) = 35.45 g/mol, z = 1. Standard: 6 mL sodium chloride solution, c(NaCl) = 0.2 g/L. Auxiliary reagent: Aq. Nitric acid solution 22%; distilled water.
Determine that the chloride content is 30.5 ppm and the srel is 4%.
Source: METTLER TOLEDO-Titration
You can use a manual glass burette to add the sodium chloride blank solution. With a slight modification, this method can be applied to the METTLER TOLEDO G20S compact titrator.
If the positive electrode material cannot be dissolved, adding a small amount of hydrogen peroxide (H2O2) (1.5% H2O2 dissolved in 22% nitric acid) to the nitric acid solution can speed up the process. The acidic leaching/dissolving of lithium cobalt oxide produces carbon dioxide gas.
The acid dissolution of the cathode material must use a fume hood. Wear gloves, goggles and lab coat. The contents of the titration beaker should be placed in the water-containing heavy metal waste.
Chinese Standard: GB/T 11064.10-2013 Lithium Carbonate, Lithium Hydroxide Monohydrate, Lithium Chloride Chemical Analysis Method Part 3: Potentiometric Titration Method for Determination of Lithium Chloride Content.
The first derivative of the titration curve and the sample 2 titration curve. Image credit: Mettler Toledo-Titration
METTLER TOLEDO instruments are used in research, scientific and quality control laboratories, as well as many other laboratories in the pharmaceutical, chemical, food and cosmetic industries. They are the global market leaders for the three most commonly used instrument groups in laboratories (such as balances, pipettes, and pH meters), and we are pioneers in the field of automated chemistry.
METTLER TOLEDO industrial solutions cover different steps in a series of manufacturing processes for many of the same customers serving the laboratory. Solutions cover everything from raw material receipt, online process control and offline packaging control to logistics and transportation. Increasingly, these solutions are fully integrated into customers' IT environments, helping them to automate their work processes.
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Last update: December 22, 2020 at 4:22 AM
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