Determination of Nitrogen Content in Nitrocellulose by 2nd Derivative Spectrophotometry
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摘要:为了准确、快速测定硝化纤维素（NC）的含氮量，将NC碱水解成NO3-和NO2-的混合溶液，采用紫外二阶导数光谱法实现了混合溶液中两组分的分离定量，并探究了碱的浓度、干扰离子和pH对NO3-和NO2-浓度测定的影响，确定了最佳实验条件。结果表明：NO3-和NO2-的混合溶液可在223nm处确定NO3-浓度，在216nm处确定NO2-浓度，达到了无需化学手段即可分离定量的目的；分别在223nm处对NO3-浓度，在216nm处对NO2-浓度与二阶导数值进行线性回归，线性关系较好。应用该方法对5组NC样品进行含氮量测定，测定结果的相对标准偏差为0.602%，加标回收率在98.7%～104.2%之间。
Abstract:In order to accurately and quickly determine the nitrogen content of nitrocellulose (NC), NC was hydrolyzed into a mixed solution of NO3- and NO2-, and the separation and quantification of two components in mixed solution was realized by UV second derivative spectroscopy. At the same time, the effects of alkali concentration, interfering ions and pH on the NO3- and NO2- concentration determination were explored, and the best experimental conditions were determined. The results show that the concentration of NO3- at 223nm and NO2- at 216nm respectively can be determined in the mixed solution. The linear regression between NO3- and NO2- concentration and second derivative value was carried out at 223nm and 216nm, respectively. Five groups of NC samples were determined by this method, the relative standard deviation of the determination results is 0.602%, and the recovery is 98.7%～104.2%.
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