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试样用王水溶解,蒸发至体积约2mL,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、砷等干扰元素,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 sample was dissolved with aqua regia, evaporated to a volume of about 2mL, extracted with hydrochloric acid, at pH = 1, orthosilicic acid and ammonium molybdate to form heteropoly silicomolybdic acid, grass and sulfur mixed acid to eliminate phosphorus, arsenic and other interfering elements, ascorbic acid reduced silicon Molybdenum heteropolyacid silicon molybdenum blue, the establishment of a spectrophotometric method for the determination of rare earth hydrogen storage alloy silicon. The method was applied to the determination of silicon in rare earth-based hydrogen storage alloy. The detection range of silicon was 0.005% ~ 0.50%, the detection limit was 0.000% and the detection limit was 0.005% (mass fraction). The detection range of silicon was covered by low, medium and high samples. The relative standard deviations (RSDs, n = 11) were 2.04% (low), 3.81% (middle) and 2.08% (high) respectively. The spiked recoveries ranged from 97.26% to 102.02%. The actual series samples of rare earth hydrogen storage alloy (K8A, TL8A, TB7A, H3A, F2A) were analyzed experimentally and the results were in agreement with the results of ICP-AES.