二阶导数光谱法测定硝化纤维素含氮量  

Determination of Nitrogen Content in Nitrocellulose by 2nd Derivative Spectrophotometry

作　　者：丁炜 赵鹏程[1] 南策 DING Wei;ZHAO Peng-cheng;NAN Ce(School of Forensic Science and Technology,Criminal Investigation Police University of China,Shenyang,110035)

机构地区：[1]中国刑事警察学院刑事科学技术学院,辽宁沈阳110035

出　　处：《火工品》2022年第5期76-80,共5页Initiators & Pyrotechnics

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NO_(3)^(-)和NO_(2)^(-)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NO_(3)^(-)和NO_(2)^(-)浓度测定的影响,确定了最佳实验条件。结果表明:NO_(3)^(-)和NO_(2)^(-)的混合溶液可在223nm处确定NO_(3)^(-)浓度,在216nm处确定NO_(2)^(-)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NO_(3)^(-)浓度,在216nm处对NO_(2)^(-)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。In order to accurately and quickly determine the nitrogen content of nitrocellulose(NC),NC was hydrolyzed into a mixed solution of NO_(3)^(-)and NO_(2)^(-),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 NO_(3)^(-)and NO_(2)^(-)concentration determination were explored,and the best experimental conditions were determined.The results show that the concentration of NO_(3)^(-)at 223nm and NO_(2)^(-)at 216nm respectively can be determined in the mixed solution.The linear regression between NO_(3)^(-)and NO_(2)^(-)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%.

关 键 词：硝化纤维素 含氮量 紫外吸收光谱 二阶导数光谱法 

分 类 号：TJ450.6[兵器科学与技术—火炮、自动武器与弹药工程]