锂离子电池用电解液中水分检测方案(卡氏水分测定)

APKF-0188er京都電子工業株式会社KYOTO ELECTRONICSMANUFACTURING CO.，LTD. APKF-0188er Application Note Moisture of electrolyte for lithium-ion battery Industry EnergyInstrument Karl Fischer Moisture TitratorMeasurement method Coulometric titration/ Direct methodStandards GB/T 19282， HG/T 4067， SJ/T 11723 1.Scope Lithium hexafluorophosphate (LiPF6) is the most popular electrolyte in lithium-ion batterieselectrolytic solution. Lithium hexafluorophosphate reacts with moisture to producehydrofluoric acid. If moisture is present in the electrolyte， its deterioration will accelerate.Therefore， it is important to measure the moisture content of the electrolyte when consideringthe long life of batteries and quality control. This application introduces an example of moisture measurement of a lithium-ion batteryelectrolyte containing lithium hexafluorophosphate. In this case， methanol-free reagent wereused， since methanol-based reagent would cause interference due to side reactions. 2. Precautions Test operation must be performed in the hood to eliminate the risk of organic solvents.It is recommended to use an electronic balance that can measure up to the order of 0.1 mg. 3. Post-measurement procedure . After thee mneasurement.hydrofluoric acidgenerated by the hydrolysisf mhexafluorophosphate causes corrosion of electrodes and flasks， and precipitation of insolublematerials. To prevent this， after the measurement， drain the reagent and wash the titration flask，twin platinum electrode and electrolytic electrode with a solvent such as toluene. 4. Apparatus Main unit：Karl Fischer Moisture Titrator (for coulometric method) Electrode： Twin platinum electrode， 2Component Inner Burette 5. Reagents ·KEMAQUA Anolyte AKE ·KEMAQUA Catholyte CGE 京都电子工业株式会社-可睦电子(上海)商贸有限公司上海市徐汇区宜山路333号1201室电话： 021-54488867 电邮： kemu-kem@163.com网址： http：//www.kem-china.com 6. Procedure -Preparation- Put approximately 5mL catholyte in the inner cell. )Prepare approximately 100mL anolyte in titration cell.23IDehydrate the measuring cell by performing pre-titration in advance. -Measurement- 1) Take the sample using a syringe and measure the mass. 2) Inject the sample to titrating cell and measure the moisture content. 3) Measure the mass of the syringe after sample injection. 4) The difference in the mass of the syringe before and after sample injection is the sampleamount. 7.Calculation Moisture content (ppm)=(Data-DriftXt-Blank)/(Wt1-Wt2)×F×1 Data Total water content after electrolysis in the titration cell (ug) Drift ·Drift level which changes by ambient moisture and carrier gaspermeating into the titration cell (ug/s) Blank ···Blank level (Opg) ..Titration time length from start to the end of titration aftersample is discharged.(s) Wt1 ··The total weight of sample and sampler before sample isdischarged. (g) Wt2 ··The total weight of sampler and sample residue after sample isdischarged. (g) F ·Compensation coefficient for calculation results (1.0) 8. Example -Parameter of titration- Titration mode ：H2O Cell type ： 2-Comp. t(stir) ： 0s Stable ： 0.1ug/s t(wait) ： 15s Control gain ： 5.0 t(max) ：0s Electrolysis speed ：standard Drift stop ： Rel. End level ： 200mV Rel. ： 0.1ug/s Start mode ： Auto Data sampling time ： 5s Stirrer speed ：3 (The above condition is an example. The setting condition depends on the titrator model.) 京都电子工业株式会社-可睦电子(上海)商贸有限公司电话： 021-54488867 电邮： kemu-kem@163.com Table 1 The measurement result Sample(g) Moisture(ug) Water content(ppm) 1 3.9166 64.1 16.37 2 3.7292 63.6 17.05 3 3.9114 66.1 16.90 Mean - 16.77 SD - 0.36 RSD(%) - - 2.13 9. Summary The RSD value (relative standard deviation) was less than 3%， and good repeatability wasobtained. Karl Fischer Moisture Titrator can be used to measure the moisture content ofelectrolytes for lithium-ion batteries. 京都电子工业株式会社-可睦电子(上海)商贸有限公司电话：021-54488867 电邮： kemu-kem@163.com / 都電子工業株式会社KYOTO ELECTRONICSMANUFACTURING CO.，LTD. 锂离子电池用电解液水分测定 应用资料(英文版)六氟磷酸锂(LiPF6)是锂离子电池电解液中最常用的电解质。六氟磷酸锂与水分反应生成氢氟酸。如果电解液中存在水分，其劣化将加快。因此，考虑到电池的寿命和质量控制，测量电解液的含水量很重要。本应用为六氟磷酸锂的锂离子电池电解液水分测量范例。在这种情况下，使用了无甲醇试剂，因为含有甲醇的试剂会因副反应而产生干扰。