离子色谱法测定石墨烯中水溶性阴离子含量  

Determination of water-soluble anions content in graphene powder by ion chromatography

作　　者：魏晓晓[1,2] 刘伟丽 王宁[3] 乐胜锋 WEI Xiaoxiao;LIU Weili;WANG Ning;LE Shengfeng(Beijing Center for Physical and Chemical Analysis,Beijing 100094,China;Beijing Key Laboratory of Detection Technology&Quality Evaluation of Organic Material,Beijing 100094,China;Metrohm China Co.,Ltd.,Beijing 100085,China)

机构地区：[1]北京市理化分析测试中心,北京100094 [2]有机材料检测技术与质量评价北京市重点实验室,北京100094 [3]瑞士万通中国有限公司,北京100085

出　　处：《中国测试》2022年第8期68-72,93,共6页China Measurement & Test

基　　金：北京市科学技术研究院北科学者计划(BS202001)。

摘　　要：建立石墨烯粉体中氟离子(F^(-))、氯离子(Cl^(-))、亚硝酸根离子(NO_(2)^(-))、溴离子(Br^(-))、硝酸根离子(NO_(3)^(-))、硫酸根离子(SO_(4)^(2-))和磷酸根离子(PO_(4)^(3-))的离子色谱分析方法。石墨烯样品冷冻研磨后,加入超纯水超声提取,过0.22μm聚醚砜滤膜,以IonPac AS11-HC阴离子色谱柱进行分离,8~40.0 mmol/L KOH淋洗液梯度洗脱,采用电导检测器检测,外标法定量。结果表明,7种阴离子的峰面积与其质量浓度在一定范围内呈现良好的线性关系,检出限和定量限分别为0.001~0.06 mg/L和0.003~0.198 mg/L,相对标准偏差为0.5%~5.7%(n=6),回收率在94.0%~104.0%之间。An ion chromatography method was developed to detect F^(-),Cl^(-),NO_(2)^(-),Br^(-),NO_(3)^(-),SO_(4)^(2-),PO_(4)^(3-)in graphene powder.Sample was dispersed in ultrapure water extracted ultrasonically after freezing grind.After extraction,two milliliter of the solution was filtered with a 0.22μm polyethersulfone filter.IonPac AS11-HC was selected as the separation column,8-40.0 mmol/L KOH solutions were used as the mobile phase in gradient elution.The constituents of sample were analyzed by a conductivity detector,and quantified by external standard method.The method showed that the peak areas of the 7 anion components presented a good linear relationship in definite range of mass concentration.The limits of detection and quantification were 0.001-0.06 mg/L and 0.003-0.198 mg/L,respectively.The recoveries of this method were in the range of 94.0%to 104.0%,with relative standard deviations ranging from 0.5%to 5.7%(n=6).

关 键 词：离子色谱法 石墨烯 阴离子 

分 类 号：O652.2[理学—分析化学] TB9[理学—化学]