摘要
建立电感耦合等离子发射光谱法(ICP–OES)测定石墨烯中铝、锰、硅、铁和钾元素的分析方法。称取0.1 g样品于铂金坩埚中,采用160℃干燥2 h、300℃灰化2 h、1000℃灼烧2 h,然后用盐酸–氢氟酸混酸溶解残留氧化物的前处理方式,采用ICP-OES法测定溶液中的5种杂质元素含量。在实验条件下,铝、锰、硅、铁和钾元素的质量浓度分别在0.5~5.0、5.0~60.0、0.5~5.0、0.1~1.5、0.1~1.5 mg/L范围内与发射强度线性关系良好,相关系数均大于0.999,检出限不大于0.003%。石墨烯中5种杂质元素含量测定结果的相对标准偏差为0.6%~9.9%(n=12),两种浓度水平的加标回收率为91%~108%,满足方法验证学的要求。该方法快速、简便、稳定性好,满足石墨烯中杂质元素含量的测定需求。
An analytical method of inductively coupled plasma emission spectrometry was established to determine aluminum,manganese,silicon,iron,and potassium in graphene.0.1 g sample was put in a platinum crucible,dried at 160℃for 2 h,ashing at 300℃for 2 h,burning at 1000℃for 2 h,and then HCl–HF mixed acid was used to dissolve the residual oxide.ICP–OES method was used to determine the content of 5 impurity elements in the sample solution.Under the experimental conditions,mass concentration of Al,Mn,Si,Fe and K had a good linear relationship with emission intensity in the range of 0.5–5.0,5.0–60.0,0.5–5.0,0.1–1.5 and 0.1–1.5 mg/L,respectively,the correlation coefficents were all more than 0.999,and the detection limits were not more than 0.003%.The relative standard deviation of the determination results of the content of 5 impurity elements in graphene was 0.6%–9.9%(n=12),and the recovery rate of the two concentration levels was 91%–108%,which meets the requirements of method validation.The method is fast,simple and stable,which meets the requirement for the determination of impurity elements in graphene.
作者
汪磊
蒙益林
耿小颖
高帅
李燕昌
颜京
WANG Lei;MENG Yilin;GENG Xiaoying;GAO Shuai;LI Yanchang;YAN Jing(AECC Beijing Institute of Aeronautical Materials,Beijing Key Laboratory of Aeronautical Materials Testing and Evaluation,Key Laboratory of Science and Technology on Aeronautical Materials Testing and Evaluation Aeroengine Corporation of China,Aviation Key Laboratory of Science and Technology on Materials Testing and Evaluation,Beijing 100095,China)
出处
《化学分析计量》
CAS
2022年第6期10-13,共4页
Chemical Analysis And Meterage
