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本文拟定钒和5-Br-PADAP——H_2O_2在1.5M磷酸介质中显色,比在硫酸或醋酸盐介质中显色的酸度大,因而选择性也明显增加。该络合物于波长590nm有最大吸收,摩尔吸光系数为4.2×10~4,络合物可稳定16小时。25ml体积中含钒0～10μg符合比尔定律。本法是将试样加热处理、酸溶、调整酸度后,直接显色测定。对四种不同钒含量的油样与不同的方法测定结果进行对照,精密度和准确度较好,最大相对偏差均在10％以下。加入回收试验,其回收率为95～103％。如取样1～5g试样时,最低下限可测至0.5～0.1ppm。本法简便、灵敏、准确,可用于石油及其渣油中微量钒的测定。
In this paper, vanadium and 5-Br-PADAP-H 2 O 2 were prepared to develop color in 1.5M phosphoric acid medium, which showed a greater acidity than sulfuric acid or acetate medium. The complex has the maximum absorption at 590nm, the molar absorptivity is 4.2 × 10 ~ 4, and the complex can be stable for 16 hours. 25ml volume containing vanadium 0 ~ 10μg in line with Bill’s law. This method is the sample heat treatment, acid-soluble, adjust the acidity, the direct color determination. The four kinds of samples with different content of vanadium were compared with the results of different methods, the precision and accuracy were better, and the maximum relative deviation was less than 10%. Add recycling test, the recovery rate of 95 ~ 103%. Such as sampling 1 ~ 5g sample, the lowest limit can be measured to 0.5 ~ 0.1ppm. This method is simple, sensitive and accurate and can be used for the determination of trace vanadium in petroleum and its residue.