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作 者:张健[1] 徐桔红 马晓蕾 孙芳 陈帅 ZHANG Jian;XU Juhong;MA Xiaolei;SUN Fang;CHEN Shuai(Taishan Fiberglass INC,Taian 271000,China;Focused Photonics(Hangzhou),Inac.,Hangzhou 310052,China)
机构地区:[1]泰山玻璃纤维有限公司,泰安271000 [2]聚光科技(杭州)股份有限公司,杭州310052
出 处:《理化检验(化学分册)》2020年第9期1030-1034,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
摘 要:采用电弧直读发射光谱法直接测定铑粉中的17种杂质元素的含量。将铑粉与缓冲剂(碳粉、碳酸锂和氟化钠按质量比7∶1∶2混合)混合研磨制备测试样品,单次样品激发时间小于1min,铑粉中17种杂质元素的最佳光谱采集时间为15~55s。17种元素的质量分数与其光谱强度分别在一定的范围内呈线性关系,方法的检出限(3s)为0.0183~1.302μg·g^-1。方法用于铑粉样品分析,加标回收率为92.2%~105%,所得日内相对标准偏差(n=5)为6.9%~19%,日间相对标准偏差(n=5)为1.5%~5.1%;测定结果与电感耦合等离子体原子发射光谱法(ICP-AES)检测结果相符。The content of 17 impurity elements in rhodium powder was determined by arc direct reading emission spectrometry.The rhodium powder was mixed and ground with buffer(toner,lithium carbonate,sodium fluoride according to 7∶1∶2 mass ratio)to prepare the test sample.The excitation time of single sample was less than 1 min,andthe optimal spectral collection time of 17 impurity elements in rhodium powder was in the range of 15-55 s.Linear relationships between mass fraction and spectral intensity of 17 elements were found in the definite ranges,with detection limit(3 s)in the range of 0.018 3-1.302μg·g^-1.The proposed method was applied to the analysis of rhodium powder sample,giving values of recovery ranged from 92.2% to 105%.Values of intra-day and inter-day RSDs(n=5)found were in the range of 6.9%-19%and 1.5%-5.1%respectively.The results obtained by this method were consistent with those of ICP-AES.
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