双抑制在线基体去除-离子色谱法测定电池级碳酸锂中痕量阴离子  

Determination of trace anions in battery-grade lithium carbonate by double-inhibition on-line matrix-removal ion chromatography

作　　者：吴刚 吴国权 WU Gang;WU Guoquan(Chia Tai Tianqing Pharmaceutical Group Co.,Ltd.,Lianyungang 222062,China;Guangzhou Application R&D Center,Thermo Fisher Technology(China)Co.,Ltd.,Guangzhou 510800,China)

机构地区：[1]正大天晴药业集团股份有限公司,江苏连云港222062 [2]赛默飞世尔科技(中国)有限公司广州应用研发中心,广东广州510800

出　　处：《色谱》2024年第3期291-295,共5页Chinese Journal of Chromatography

摘　　要：建立了一种测定电池级碳酸锂中痕量阴离子的方法。用超纯水超声辅助溶解碳酸锂,采用在线基体去除法去除碳酸锂基体,基体去除过程中,样品首先流入到ADRS600(4 mm)抑制器(抑制电流150 mA,抑制器再生液外接水流速2 mL/min)中,在抑制器内通过离子交换膜作用,碳酸锂中的锂离子与氢离子置换,碳酸锂变成碳酸;然后经过CRD 200(4 mm),碳酸以二氧化碳的形式排出离子色谱系统,从而达到去除碳酸锂基体的目的;最后待分析阴离子被自动富集在IonPac UTAC-LP2浓缩柱(35 mm×3 mm)上,通过阀切换技术将阴离子自动转移到色谱分析系统中。在色谱分析系统中,以IonPac AG18(50 mm×2 mm)为保护柱,IonPac AS18(250 mm×2 mm)为分析柱,柱温箱为30℃,KOH溶液为淋洗液进行梯度洗脱,泵流速0.30 mL/min,抑制器为ADRS600(2 mm),抑制电流25 mA,进样体积为250μL,检测器为电导检测器。结果显示:F^(-)、Cl^(-)、NO_(2)^(-)、Br^(-)、NO_(3)^(-)及SO_(4)^(2-)离子在各自的线性范围内具有良好的线性关系(r≥0.999);各离子的检出限和定量限分别为0.05~0.88μg/L和0.15~2.92μg/L;碳酸锂样品连续6针进样各离子峰面积的相对标准偏差(RSD)均≤0.73%;同一碳酸锂样品处理完后分别放置0、2、4、8、12、18、24 h后进样,各离子峰面积的RSD均≤0.96%;在3个添加水平下,各离子加标回收率为93.3%~99.3%,RSD(n=6)为0.97%~3.45%;本方法具有方法定量限低(各离子定量限均为0.5 mg/kg)及多种离子同时分析的优势,适用于电池级碳酸锂中痕量阴离子的检测。A method was developed for the determination of trace anions in battery-grade lithium carbonate.In this method,lithium carbonate was dissolved in ultrapure water with ultrasound assistance,and its matrix was removed using an on-line matrix-removal method.In the matrix-removal process,the sample was first passed through an ADRS600(4 mm)suppressor(suppressor current,150 mA;external water flow rate,2 mL/min).Hydrogen and lithium ions were then completely exchanged via the ion-exchange membrane in the suppressor,converting the lithium carbonate into carbonic acid.The carbonic acid entered the waste-liquid channel in the form of carbon dioxide through a CRD 200(4 mm)carbonate removal device to remove the lithium carbonate matrix.Finally,the target anions were automatically enriched on an IonPac UTAC-LP2 concentration column(35 mm×3 mm)and automatically transferred to a chromatographic system using valve-switching technology.The chromatographic system featured an IonPac AG18 column(50 mm×2 mm)as the protection column and an IonPac AS18 column(250 mm×2 mm)as the analytical column.The column temperature was 30℃,gradient elution was performed using KOH solution as the eluent,and the pump flow rate was 0.30 mL/min.An ADRS600(2 mm)suppressor,suppressor current of 25 mA,injection volume of 250μL,and conductance detector were also used.The results showed good linear relationships(r≥0.999)for F^(-),Cl^(-),NO_(2)^(-),Br^(-),NO_(3)^(-),and SO_(4)^(2-)in their respective concentration ranges.The limits of detection(LODs)and quantification(LOQs)were 0.05-0.88 and 0.15-2.92μg/L,respectively.Lithium carbonate samples were tested six consecutive times,and the relative standard deviations(RSDs)of the peak areas of each ion were less than 0.73%.The same lithium carbonate samples were injected after 0,2,4,8,12,18,and 24 h,and the RSD of the peak areas of each ion was less than 0.96%.The average recoveries ranged from 93.3%to 99.3%,and the RSDs(n=6)of samples spiked at three levels were in the range of 0.97%-3.45%.The proposed m

关 键 词：离子色谱 阴离子 碳酸锂 在线基体去除 双抑制 

分 类 号：O658[理学—分析化学]