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目的:建立抑制离子色谱法测定碳酸锂原料药中氯化物及硫酸盐的含量。方法:用Thermo Ion Pac AS11(250 mm×4mm)阴离子交换柱和Ion Pac AG 11(50 mm×4 mm)保护柱,淋洗液为10 mmol·L-1氢氧化钾溶液,由自动淋洗液发生器产生,流速为1.0 ml·min-1,柱温30℃,电导池温度35℃,阴离子抑制器抑制器电流36 m A,进样量10μl。结果:氯离子及硫酸根离子在1.0~20μg·ml-1范围内线性关系良好(r分别为0.995 1,0.997 3),氯离子回收率为106.6%(RSD=2.6%,n=6),硫酸根离子回收率为100.3%(RSD=1.9%,n=6)。结论:该方法准确可靠,可用于碳酸锂原料药中氯化物及硫酸盐的测定。
Objective: To establish a method for the determination of chloride and sulfate in raw materials of lithium carbonate by ion chromatography. Methods: The column was eluted with 10 mmol·L-1 potassium hydroxide solution using a Thermo Ion Pac AS11 (250 mm × 4 mm) anion exchange column and Ion Pac AG 11 (50 mm × 4 mm) Liquid generator, flow rate of 1.0 ml · min-1, column temperature 30 ℃, temperature of the cell 35 ℃, anion suppressor current 36 m A, the injection volume 10μl. Results: The calibration curves of chloride ion and sulfate ion in the range of 1.0 ~ 20μg · ml-1 were good (r = 0.995 and 0.9973 respectively), and the recovery of chloride ion was 106.6% (RSD = 2.6%, n = 6) Sulfate ion recovery was 100.3% (RSD = 1.9%, n = 6). Conclusion: The method is accurate and reliable and can be used for the determination of chloride and sulfate in raw materials of lithium carbonate.