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离子色谱法测定石墨烯中水溶性阴离子含量

115    2022-09-15

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作者:魏晓晓1,2, 刘伟丽1,2, 王宁3, 乐胜锋1,2

作者单位: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


关键词:离子色谱法;石墨烯;阴离子


摘要:

建立石墨烯粉体中氟离子(F)、氯离子(Cl)、亚硝酸根离子(NO2)、溴离子(Br)、硝酸根离子(NO3)、硫酸根离子(SO42–)和磷酸根离子(PO43–)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0.22 μm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。


Determination of water-soluble anions content in graphene powder by ion chromatography
WEI Xiaoxiao1,2, LIU Weili1,2, WANG Ning3, LE Shengfeng1,2
1. Beijing Center for Physical and Chemical Analysis, Beijing  100094, China;
2. Beijing Key Laboratory of Detection Technology & Quality Evaluation of Organic Material, Beijing 100094, China;
3. Metrohm China Co., Ltd., Beijing 100085, China
Abstract: An ion chromatography method was developed to detect F, Cl, NO2, Br, NO3, SO42–, PO43– 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 0.22 μm 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).
Keywords: ion chromatography;grapheme;inion
2022, 48(8):68-72,93  收稿日期: 2021-04-20;收到修改稿日期: 2021-07-26
基金项目: 北京市科学技术研究院北科学者计划(BS202001)
作者简介: 魏晓晓(1986-),女,河北沧州市人,博士,研究方向为食品接触材料安全性
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