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研究了Mo(Ⅵ)与Tiron的反应,发现在pH4.0的HAc-NaAc介质中形成1:1配合物,该配合物在252nm、315nm有两个吸收峰,而在可见光区无吸收峰。测得ε252=6.9×10 ̄3L·mol-1·Cm-1,ε315=3.5×103L·mol-1·Cm-1。据此建立了测定Mo(Ⅵ)的方法,在252nm和315nm处的线性范围分别为1.6×10-6mol·L-1~2.O×10-4mol·L-1和3.2×10-4mol·L-1~2.0×10-4mol·L-1。检出限分别为8.O×10-7mol·L-1和1.6×10-6mol·L-1.PO_4 ̄3+、SiO_3 ̄2-对测定无干扰,而W(Ⅵ)、V(Ⅴ)、Fe(Ⅲ)等有干扰。该法试用于有机磷合钼聚多酸盐样品的测定,结果满意,方法回收率96%~102%,变异系数≤1.l%(n=12)。
The reaction of Mo (Ⅵ) with Tiron was studied. It was found that 1: 1 complex was formed in HAc-NaAc medium at pH4.0. The complex has two absorption peaks at 252nm and 315nm and no absorption peak in the visible region. Ε252 = 6.9 × 10 -3 L · mol -1 · cm -1 and ε 315 = 3.5 × 103 L · mol -1 · cm -1 were measured. The method for the determination of Mo (Ⅵ) has been established. The linear range at 252 nm and 315 nm is 1.6 × 10 -6 mol·L -1. O × 10-4mol·L-1 and 3.2 × 10-4mol·L-1 ~ 2.0 × 10-4mol·L-1. Detection limits were 8. O × 10-7mol·L-1 and 1.6 × 10-6mol·L-1. PO_4 ~ 3 +, SiO_3 ~ 2-no interference on the determination, and W (Ⅵ), V (Ⅴ), Fe (Ⅲ) and other interference. The method was applied to the determination of organophosphorus molybdenum polyacid samples with satisfactory results. The method recoveries ranged from 96% to 102% and the coefficients of variation were ≤1. l% (n = 12).