化工原料及制药中间体中二苯胺亚硝化衍生的极谱法测定

Polarographic Determination of Diphenylamine Nitroation in Industrial Raw Material and Pharmaceutical Intermediater

报道一种经亚硝化后用极谱定量二苯胺的极谱测定方法。在０．２ｍｏｌ／ＬＨＡｃ－０．０２５ｍｏｌ／ＬＨ＿２ＳＯ＿４－４×１０￣（－６）ｍｏｌ／ＬＮａＮＯ＿２底液中，二苯胺的亚硝化产物有一良好的极谱还原波，峰电位为－０．６１Ｖ（ｖｓ，ＳＣＥ），峰高与二苯胺浓度在２×１０￣（－７）～１×１０￣（－５）ｍｏｌ／Ｌ范围内有线性关系（ｒ＝０．９９９９）。

A method for the determination of diphenylamine (Ⅰ)is reported based on the nitrosation ofIand the subsequent polarographic measurement of N-nitroso-Ⅰ. In 0. 2 mol/L HAc-0. 025 mol/LH_2SO_4-4 × 10￣(-6)(or 4 × 10￣(-5))mol/L NaNO_2 medium,N-nitroso-Ⅰ yields a well-difined reductionwave with a peak potentiaI Ep-0.61 V(vs,SCE). The peak height is linear proportional to the con-centration of I in the range from 2 × 10￣(-7)mol/L to 1 × 10￣(-5)mol/L(γ=0. 9999). The method has beenapplied to the determination of the content of I in industrial raw material and pharmaceutic intermedi-arer.