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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) method for the determination of NdFeB alloy main elements of large fluctuations, the relative standard deviation is usually as high as 0.5%, seriously affecting the composition of different grades of NdFeB magnets and performance control. In order to solve this problem, the inductively coupled plasma atomic emission spectrometry (ICP-AES) was used to determine the three main elements of Nd, Fe and B in NdFeB alloys simultaneously with high accuracy. The appropriate analytical line was selected and the background subtracted. By using matrix matching, optimizing instrument parameters, maintaining a stable ICP torch, correcting peak drift (using software calibration function, correcting drift of each element, correcting the original test data after correction), etc., NdFeB main elements of high-precision test. The results showed that the short-term relative standard deviations of Nd, Fe and B were 0.09%, 0.04% and 0.31%, respectively, and the recoveries were 97% -103%. The relative standard deviations for long-term were 0.17% , 0.08% and 0.52%, respectively. The same synthetic samples were tested. The relative deviation between ICP and XRF was less than 1%, and the relative deviation from ICP was less than 0.1% Spectrophotometry and ICP measurements of foreign laboratories The results of the control to meet the production, scientific research requirements.