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作 者:刘晓杰[1,2,3] 王燕霞 于勇海[1,2,3] LIU Xiao-jie;WANG Yan-xia;YU Yong-hai(Baotou Research Institute of Rare Earths,Baotou 014030,China;Ruike National Engineering Research Center of Rare Earth Metallurgy and Function Materials,Baotou 014030,China;State Key Laboratory of Baiyunebo Rare Earth Resource Researches and Comprehensive Utilization,Baotou 014030,China;Baotou Light Industry Vocational Technical College,Baotou 014035,Chin)
机构地区:[1]包头稀土研究院,内蒙古包头014030 [2]稀土冶金及功能材料国家工程研究中心,内蒙古包头014030 [3]白云鄂博稀土资源研究与综合利用国家重点实验室,内蒙古包头014030 [4]包头轻工职业技术学院,内蒙古包头014035
出 处:《冶金分析》2018年第3期51-55,共5页Metallurgical Analysis
摘 要:采用王水分解样品,在3%(V/V)的盐酸介质中,以标准加入法绘制校准曲线,建立了空气-乙炔火焰原子吸收光谱法(FAAS)测定钐钴永磁合金中钙的方法。分别在钐、钴单独存在以及共同存在的条件下考察了其对测定的影响,结果表明,若采用火焰原子吸收光谱法测定钐钴永磁合金中钙,钐钴基体对测定的基体效应不可忽略且情况复杂。因此,实验选择标准加入法来校正钐钴基体效应对测定的影响。方法检出限为13μg/g,方法测定下限为44μg/g。干扰试验表明,以标准加入法的校正模式进行钐钴永磁合金中钙量的测定,样品中共存元素铜、铁、锆对测定的干扰可忽略。方法应用于钐钴永磁合金中实际样品中质量分数为0.006 5%钙的测定,测定值与国家标准方法 GB/T 12690.15—2006(电感耦合等离子体原子发射光谱法)相符,测定结果的相对标准偏差(RSD,n=11)小于14%。方法可用于钐钴永磁合金样品中0.005 0%~0.50%(质量分数)钙量的分析检测。The sample was decomposed with aqua regia.The calibration curve was prepared by standard addition method in 3%(V/V)hydrochloric acid medium.A determination method of calcium in samarium-cobalt permanent magnet alloy by air-acetylene flame atomic absorption spectrometry(FAAS)was established.The influence of samarium and cobalt on determination was investigated whether samarium and cobalt exist single or together.The results showed that the matrix effect of samarium and cobalt was complex and could not be ignored if the content of calcium in samarium-cobalt permanent magnet alloy was determined by flame atomic absorption spectrometry.Therefore,the standard addition method was used to correct the influence of matrix effect of samarium and cobalt on determination.The detection limit of method was 13μg/g.The low limit of determination was 44μg/g.The interference tests indicated that the interference of coexisting elements in sample including copper,iron and zirconium could be ignored when the content of calcium in samarium-cobalt permanent magnet alloy was determined by correction mode of standard addition method.The proposed method was applied for determination of calcium with mass fraction of 0.006 5%in actual sample of samarium-cobalt permanent magnet alloy.The results were consistent with those obtained by national standard method,i.e.,GB/T 12690.15-2006(inductively coupled plasma atomic emission spectrometry).The relative standard deviation(RSD,n=11)of determination results was less than 14%.The proposed method could be used for the analysis of calcium with mass fraction in range of 0.005 0%-0.50%in samarium-cobalt permanent magnet alloy sample.
关 键 词:空气-乙炔火焰 火焰原子吸收光谱法(FAAS) 钐钴永磁合金
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