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本文提出在磷酸介质中以5-Br-PADAP直接分光光度法测定合金钢和高温合金中铌。选用柠檬酸和EDTA二钠盐为掩蔽剂,用氟化物使络合物褪色的溶液作参比液以消除共存元素及基底的影响。铌量在0—30μg/50mL范围内遵守比尔定律。依据铌的标准加料回收试验和标样分析结果计算测定误差小于4.6%本方法灵敏度高(ε=5.1×10~4),并已应用于合全钢和高温合金中铌的测定。测定下限为5×10~(-3)%。
This paper presents the determination of niobium in alloy steel and superalloy by 5-Br-PADAP direct spectrophotometry in phosphoric acid medium. Selection of citric acid and EDTA disodium salt as masking agent, fluoride complex fading solution as a reference solution to eliminate the impact of coexisting elements and substrates. Beer’s law is obeyed in the range of 0-30μg / 50mL niobium. The method has good sensitivity (ε = 5.1 × 10 ~ 4) and has been applied to the determination of niobium in all-steel and superalloy based on the standard addition recovery test of niobium and the standard analysis results. The lower limit of determination is 5 × 10 -3%.