Abstract:The sample was dissolved with sulfuric acid and nitric acid. The ammonium nitrate solution was added into sample solution to dissolve the salts formed in treatment process and to prevent the hydrolysis of niobium, tungsten and zirconium. Under the optimized instrumental operation conditions, the content of niobium, tungsten and zirconium in sample solution was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). Consequently, the determination method of niobium, tungsten and zirconium in steel was established. The researches indicated that 0.1 g of steel sample could be dissolved in 15 mL of sulfuric acid and several drops of nitric acid by heating and the salts formed after fumes of sulfuric acid to be evolved could be completely dissolved by adding 10 mL of 4.0 g/L ammonium nitrate solution. Nb 316.340 nm, Zr 343.823 nm and W 207.011 nm were selected as the analysis lines. The matrix interference was eliminated by matrix matching method. The correlation coefficients of calibration curves of testing elements were all higher than 0.999 5. The detection limits of niobium, tungsten and zirconium were 1.9, 9.9 and 3.2 ng/mL, respectively. The proposed method was applied to the determination of niobium, tungsten and zirconium in YSBC11217-94 low alloy steel standard sample. The found results were consistent with the certified values. The relative standard deviation (RSD, n=10) was 1.7%, 1.1% and 2.1%, respectively. The recoveries of standard addition were between 97% and 104%. The content of niobium, tungsten and zirconium in other standard samples (including middle alloy steel, structural alloy steel and low alloy steel) and synthetic steel samples was determined. The found results were consistent with the certified values or reference values.
杨丽荣,于媛君,亢德华,顾继红,顾兰兰,王铁. 电感耦合等离子体原子发射光谱法测定钢中铌钨锆[J]. 冶金分析, 2014, 34(11): 51-55.
YANG Li-rong, YU Yuan-jun, KANG De-hua,GU Ji-hong,GU Lan-lan, WANG Tie. Determination of niobium,tungsten and zirconium in steel by inductively coupled plasma atomic emission spectrometry. , 2014, 34(11): 51-55.