摘要:
研究了应用二安替比林甲烷 (DAPM) 分光光度法测定氮化硅铁中钛元素含量的分析方法, 通过对试样分解方法、硫酸冒烟、显色条件、干扰及消除方法等的试验研究, 确定了最佳分析条件。试样采用3 g氢氧化钠熔剂于铁坩埚中在650℃下熔融分解, 熔块以50 mL热水浸取, 再以10 mL盐酸、5 mL氢氟酸酸化, 然后以7 mL硫酸分两次冒烟除去硅和多余的氢氟酸。以抗坏血酸还原Fe (Ⅲ) 离子消除铁的干扰, 再在室温下2 mol/L的盐酸介质中与二安替比林甲烷反应显色, 最后于吸收波长390 nm处进行测定。试验测得该方法的检测限为0.02%, 将其应用于氮化硅铁标准样品的测定, 结果显示, 在0.05%~2.0%含量范围内该方法具有良好的准确度和精密度。
Abstract:
A method for determination of titanium content in ferrosilicon nitride by diantipyrylmethane(DAPM) spectrophotometry was investigated.Some condition experiments were done,which includes decomposition of samples,smoking of sulfuric acid,coloring,interference and eliminating method,and the optimal conditions were obtained.The sample was fused and decomposed with 3 g sodium hydroxide in an iron crucible at 650 ℃.The sintered mass was dissolved with 50 mL hot water,and then the solution was acidified with 10 mL hydrochloric acid and 5 mL hydrofluoric acid. The silicon and residual hydrofluoric acid in the solution was removed by total 7 mL sulfuric acid for two times of smoking.The Fe (Ⅲ) ion was reduced by ascorbic acid to eliminate the interference of iron in the solution.After the reaction with diantipyrylmethane in 2 mol/L hydrochloric acid medium at room temperature,the solution was measured at absorption wavelength of 390 nm by photometer.A detection limit of 0.02% for this method was also obtained by experiments.At last,this method was applied to the determination of some ferrosilicon nitride standard samples,good accuracy and precision were evidenced with 0.05%~2.00% of titanium content.