ICP-AES法测定碳钢、低合金钢中13种元素

本文选择了硝酸、王水、逆王水,进行碳钢、低合金钢溶样条件试验,以谱线强度为指标,溶解酸种类、溶解酸浓度、溶解酸用量、定容酸用量等四因素为变化条件,各因素中有三水平,即按正交实验表L_9(3~4)进行试验,编制计算程序,快速、科学地优选出最佳溶样条件—30ml NHO_3(1+5v/v)和3ml HCl,ICP-AES法同时测定铝、砷、铬、钴、铜、磷、锰、钼、镍、硅、锡、钛和钒13种元素。为确定测试方法的重复性(r)和再现性(R)而进行精密度试验。精密度数据是由10个实验室对7个样品作试验确定的。方法的回收率为94％-105％。精密度在8％以内。

Determination of Trace Al, As, Co, Cr, Cu, Mn, Mo, Ni, P, Si, Sn, Ti, and V Content of Carbon Steel and Low Alloyed Steel by ICP-AES Method

Nitric acid, aqua regia, and counter aqua regia were selected for engaging in the carbon steel and low alloyed steel sample dissolution experiment. The spectral intensity was taken as index. The four factors-kinds of dissolution acids, its concentration, used volume, and amount of acid used for volume graduating-were taken as variables. There were three levels for each factor, it means, the experiments were processed and calculation program was worked out according to orthogonal design form L9 (34). The best conditions of sample dissolution were selected fast and scientifically. It was 30mL HNO3 (l 5v/v), 3mL HC1. The aluminium, arsenic, chromium, cobalt, copper, phosphorus, manganese, molybdenum, nickel, silicon, tin, titanium, and vanadium thirteen elements'content was simultaneously determined by ICP-AES method. Seven levels were selected. The repeatability (r) and reproducibility (R) were defined by cooperative test of ten laboratories. The recovery was 94%-105%.The precision was within 8%.