电感耦合等离子体原子发射光谱法测定铁镍钴系非晶合金中高含量钴、铌、硼和铜含量

Determination of cobalt,niobium,boron,copper and in FeNiCo amorphous alloy by inductively coupled plasma atomic emission spectrometry

建立了电感耦合等离子体原子发射光谱法(ICP-AES)同时测定铁镍钻系非晶合金中高含量钴、铌、硼和铜元素的分析方法。采用王水、氢氟酸、甘露醇、硫磷酸,并在聚四氟乙烯烧杯中溶解样品,避免了溶祥不完全和过程中引入待测元素硼;采用铁镍基体匹配结合标准溶液制作校准曲线从而消除了基体干扰;测定过程采用钇元素内标法,优选了待测元素和内标元素分析谱线,确定了校准曲线及ICP光谱仪工作条件,消除了光谱干扰并提高了方法精密度水平。在仪器工作条件下,各元素校准曲线线性相关系数均大于0.9995。方法精密度结果的相对标准偏差(RSD,n=10)在0.43%~1.47%之间,回收率97%~104%,测定结果与化学分析方法的测定结果一致。

A method for simultaneous determination of cobalt,niobium,boron and copper in FeNiCo amorphous alloy by inductively coupled plasma atomic emission spectrometry(ICP-AES)was established.Hydrochloric acid and nitric acid,hydrofluoric acid,mannitol and thiophosphoric acid were used to dissolve the sample in a Teflon beaker to avoid incomplete dissolution and the introduction of boron in the process.FeNi matrix was used to match the calibration curve with standard solution to eliminate matrix interference;yttrium internal standard method was used in the detennination process to optimize the analytical spectral lines of the elements to be determined and internal standard elements,and determine the calibration curve The spectral interference was eliminated and the precision of the method was improved.Under the working conditions of the instrument,the linear correlation coefficients of the calibration curves of each element are greater than 0.9995.The relative standard deviation(RSD,n=10)of the precision of the method was between 0.43%and 1.47%,and the recovery was 97%to 104%.The results were consistent with those of chemical analysis.