ICP-AES法高精度测定钕铁硼合金中主量元素  

Determination of Main Components in Nd-Fe-B Alloy with High Precision by Inductively Coupled Plasma Atomic Emission Spectrometry

作　　者：徐静[1] 李明来[1] 李世鹏[1] 彭海军[1] 赵斌[1] 于敦波[1] 

机构地区：[1]北京有色金属研究总院稀土材料国家工程研究中心 有研稀土新材料股份有限公司,北京100088

出　　处：《中国稀土学报》2014年第2期234-239,共6页Journal of the Chinese Society of Rare Earths

摘　　要：电感耦合等离子体原子发射光谱（ICP—AES）法测定钕铁硼合金主量元素波动大，相对标准偏差通常高达0．5％以上，严重影响不同牌号钕铁硼磁体的成分配比与性能控制。为了解决这一难题，本文研究了电感耦合等离子体原子发射光谱法同时高精度测定钕铁硼合金中Nd，Fe，B三种主量元素，选择了合适的分析线并扣除了背景。通过采用基体匹配、优化仪器参数、保持稳定的ICP焰炬、校正谱峰漂移（采用软件的校正功能，对各元素进行漂移校正，校正完成后，对原测试数据进行再处理）等，实现了对钕铁硼主量元素的高精密度测试。结果表明：Nd，Fe，B三种元素的短期相对标准偏差分别为：0．09％，0．04％，0．31％，加标回收率为97％～103％；5天内的长期相对标准偏差为：0．17％，0．08％，0．52％；测试同一合成样品，ICP测定值与x射线荧光光谱法测定值相对偏差小于1％，与国外实验室ICP法的测定值相对偏差小于0．1％，测定值与x射线荧光光谱法和国外实验室ICP法的测定值对照结果满足生产、科研的测定要求。Inductively coupled plasma atomic emission spectrometry（ICP-AES） has a disadvantage of big deviation in testing the content of main elements in NdFeB alloy, its relative standard deviation is often as high as 0.5% above, which seriously impacts on component proportion and performance control of different types of NdFeB magnet. In order to solve this problem, a method of simultaneous determination of neodymium, iron and boron in Nd- Fe-B alloy with high precision by inductively coupled plasma atomic emission spectrometry was studied in this paper. The suitable analytical lines were selected with deduction of the background. The high-precision determination of Nd-Fe-B alloy was realized by using matrix matching, optimizing instrument parameters, keeping stable ICP torch flame and correcting spectral peak drift（ It is necessary to deal with the drift correction of each element with the correction function of software, and then to process the original test data again）, etc.. The results showed that the short-term relative standard deviations of Nd, Fe, and B were 0.09%, 0.04%, 0.31% with the recovery rate between 97% to 103%, and the long relative standard deviations in five days were 0.17%, 0.08% , 0.52%, respectively. Testing the same synthetic samples, the relative deviation of value determined between ICP and X-ray fluorescence spectrometry was less than 1% , while less than 0.1% between ICP in this paper and foreign laboratoties＇ ICP method. It could be seen that the determinations of Nd, Fe and B elements were consistent with those by X-ray fluorescence spectrometry and ICP method of foreign laboratories, which could meet the testing requirements of the production and scientific research

关 键 词：ICP—AES 高精度 钕铁硼合金 主量元素 

分 类 号：O657.31[理学—分析化学]