摘要
试验用10 mL(1+1)硝酸溶解样品,选择Si 251.611 nm、Cu 324.754 nm、P 178.284 nm、As 189.042 nm、Pb220.353 nm、Sn 189.989 nm,Sb 206.833 nm为分析线,干扰系数法消除共存元素光谱干扰,采用钼铁标准样品绘制工作曲线,结合在线标准加入砷、铅、锡、锑元素混合标准溶液实现基体在线匹配,使用电感耦合等离子体原子光谱法(ICP-AES)测定了钼铁中硅、铜、磷、砷、铅、锡、锑元素含量。方法中各元素校准曲线线性关系良好,相关系数均不小于0.999;各待测元素的检出限为0.000 3%~0.007 2%。按照实验方法测定钼铁国际标准样品NoF17/3中硅、铜、磷、砷、铅、锡、锑,结果的相对标准偏差(RSD,n=11)在0.87%~6.05%之间,测定结果与认定值相吻合。对钼铁标准样品的加标回收率在96.8%~113.6%之间。
The sample was dissolved with 10 mL nitric acid( 1 + 1 ) . Si 251.611 nm, Cu 324.754 nm, P 178.284 nm, As 189.042 nm, Pb 220.353 nm, Sn 189.989 nm and Sb 206.833 nm were selected as analytical lines. The spectral in-terference could be well corrected by interference method. The standard solution series were prepared by matrix matc-hing method and 7 elements mixed standard solution on line for the plotting of calibration curve. The content of 7 ele-ments in ferromolybdenum (including silicon, copper, phosphorus, arsenic, lead, tin and antimony) was determined by inductively coupled plasma atomic emission spectrometry(ICP-AES) . The linearity of calibration curve for each ele-ment was good with correlation coefficient higher than 0.999. The detection limits of elements were between 0.000 3 % and 0.007 2% . The content of silicon, copper, phosphorus, arsenic, lead, tin and antimony in NoF17/3 standard fer-romolybdenum sample was determined according to the experimental method. The relative standard deviations ( RSD, n = ll) were between 0.87% and 6.05% . The determination results of standard sample were consistent with the certi-fied values. The recoveries for standard samples of ferromolybdenum were between 96.8% and 113.6% .
出处
《铁合金》
2017年第8期44-48,共5页
Ferro-alloys