材料期刊网

试样用王水溶解,蒸发至体积约2 mL,盐酸提取,在pH=1时,正硅酸与钼酸铵形成硅钼杂多酸,草硫混酸消除磷、砷等于扰元素,抗坏血酸还原硅钼杂多酸为硅钼蓝,建立了分光光度法测定稀土系贮氢合金中硅的方法.方法用于稀土系贮氢合金中硅的测定,硅的检测范围为0.005 0％～0.50％,检出限为0.000 50％,检测下限为0.005 0％(质量分数).方法中用低、中、高三个样品涵盖硅的检测范围,结果的相对标准偏差(RSD,n=11)分别为2.04％(低),3.81％(中)、2.08％(高).加标回收率为97.26％～102.02％.按实验方法对稀土系贮氢合金实际系列样品(K8A、TL8A、TB7A、H3A、F2A)进行分析,结果与使用电感耦合等离子体原子发射光谱法的测定结果一致.

The samples were dissolved by aqua regia and evaporated to about 2 mL of the volume.Hydrochloric acid was extracted.The silicon molybdenum heteropoly acid was formed with silicon and ammonium molybdate at pH=1.Phosphorus and arsenic were masked with oxalic acid.The determination method of silicon in rare earth system hydrogen alloys by silicon molybdenum blue spectrophotometery was established after being reduced to silicon molybdenum blue with ascorbic acid.The proposed method was applied to the determine silicon in rare earth system hydrogen alloys.The detection range of silicon is 0.0050 ％-0.50 ％.The detection limit and lower limit of silicon in the method was 0.000 50％ and 0.005 0％ (mass fraction),Method with low,medium and high grade three samples covering the detection range of silicon.The relative standard deviations(RSD,n =11) of found results was 2.04％ (low),3.81 ％ (medium),2.08 ％ (high).The recoveries were between 97.26 ％-102.02 ％.The content of silicon in rare earth system hydrogen alloys actual sample was determined according to the experimental method,and the found results were consistent with consistent with those obtained by inductively coupled plasma atomic emission spectrometry.