微波消解-电感耦合等离子体原子发射光谱法测定高镍铸铁中硅锰磷铬镍铜

目前髙镍铸铁已广泛用于汽车发动机等产品上,对于材料中各元素的分析,传统化学分析方法已无法满足快速检测的需求。试验探讨了不同溶解方式的溶样效果,优选了王水并采用微波消解,冷却后在消解液中滴加氢氟酸的溶解方法,测定过程采用钇内标法进行检测,从而实现了使用电感耦合等离子体原子发射光谱法(ICP-AES)同时测定高镍铸铁中硅、锰、磷、铬、镍、铜等元素的方法。在选定的仪器工作条件下,各元素的校准曲线线性相关系数均大于0.9999,各元素的检出限为0.0002%~0.0036%。实验方法用于高镍铸铁实际样品中硅、锰、磷、铬、镍、铜的测定,结果的相对标准偏差(RSD,n=8)为0.73%~5.0%;按照实验方法测定髙镍铸铁标准样品中硅、锰、磷、铬、镍、铜,结果与认定值相吻合。

Determination of silicon,manganese, phosphorus,chromium, nickel and copper in high nickel cast iron by inductively coupled plasma atomic emission spectrometry after microwave digestion

At present, the high nickel cast iron had been widely used in many products such as automobile engine. For the analysis of elements in materials, the traditional chemical analysis method hardly meets the requirements of rapid detection. The effect of various dissolving methods was investigated. The optimum solvent for microwave digestion was aqua regia. Hydrofluoric acid was dripped in digestion solution after cooling. The yttrium internal standard method was employed in the determination process. The simultaneous determination of silicon, manganese, phosphorus, chromium, nickel and copper in high nickel cast iron by inductively coupled plasma atomic emission spectrometry (ICP-AES) was realized. Under the selected instrumental conditions, the linear correlation coefficients of calibration curves were all higher than 0.9999. The detection limits of elements were in range of 0.0002%-0.0036%. The proposed method was applied for the determination of silicon, manganese, phosphorus, chromium, nickel and copper in actual high nickel cast iron sample, and the relative standard deviations (RSD, n=8) of measured results were between 0.73% and 5.0%. The contents of silicon, manganese, phosphorus, chromium, nickel and copper in standard sample of high nickel cast iron were determined according to the experimental method, and the found results were consistent with the certified values.