离子色谱法测定废旧锂电池湿法浸出液中氟和氯

建立了离子色谱法同时测定废旧锂电池湿法浸出液中氟和氯含量的方法。以高沸点硫酸为蒸馏介质,在160~180 ℃下以水蒸气蒸馏法分离富集浸出液中氟化物和氯化物并被氢氧化钠吸收液吸收,可消除浸出液中有机物及大量共存金属离子对测定的干扰。吸收液经0.22 μm微孔滤膜过滤,并用4.5 mmol/L 碳酸钠-1.0 mmol/L 碳酸氢钠混合溶液淋洗,高容量AS23型阴离子分析柱分离,电导检测器对其检测。实验表明,氟和氯离子质量浓度在0.1~10.0 mg/L与其对应的峰面积呈良好的线性关系,线性相关系数分别为0.999 8和0.999 6。方法用于废旧锂电池湿法浸出液中氟和氯的测定,加标回收率分别为95.47%和96.29%,相对标准偏差（RSD, n=10）分别为2.9%和3.7%,结果满意。

Determination of fluorine and chlorine in leaching solution in waste lithium battery by ion chromatography

An method for simultaneous determination of fluorine and chlorine in leaching solution in waste lithium battery by ion chromatography was established.The fluorine and chlorine were separated and enriched by water steam distillation method at 160~180 ℃ with high-boiling sulfuric acid as distillation medium and absorbed by sodium hydroxide absorption solution, which could eliminate the interference caused by organic compounds and coexisting metal ions in the leaching solution.After passing through the 0.22 μm filter membrane,the fluorine and chlorine in absorption solution were separated with high-capa-city AS23 type anion analytical column and detected by conductivity detector using the mixture solution of 4.5 mmol/L Na ₂CO₃-1.0 mmol/L NaHCO₃ as eluent.The results showed that the fluorine and chlorine showed a good linear correlation with their corresponding peak areas in the concentration range of 0.1~10.0 mg/L with correlation coefficient of 0.999 8 and 0.999 6,respectively.The proposed method was applied to the determination of fluorine and chlorine in leaching solution in waste lithium battery with satisfactory results,registering the standard addition recovery of 95.47% and 96.29% with the relative standard deviations（RSD, n=10） of 2.9% and 3.7%, respectively.The result was satisfactory.