紫外分光光度计法测定硝化纤维素含氮量  

Determination of Nitrogen Content of Nitrocellulose by Ultraviolet Spectrophotometer

作　　者：薛会会 黄娟 张阿磊[3] 陈可泉 周杰[1,2] 丁亚军 肖忠良[1,2] XUE Hui-hui;HUANG Juan;ZHANG A-lei;CHEN Ke-quan;ZHOU Jie;DING Ya-jun;XIAO Zhong-liang(School of Chemistry and Chemical Engineering,Nanjing University of Science and Technology,Nanjing 210094,China;Key Laboratory of SpecialEnergy Materials,Ministry of Education,Nanjing University of Science and Technology,Nanjing 210094,China;College of Biotechnology andPharmaceutical Engineering,Nanjing Technology University,Nanjing 211816,China)

机构地区：[1]南京理工大学化学与化工学院,江苏南京210094 [2]南京理工大学特种能源材料教育部重点实验室,江苏南京210094 [3]南京工业大学生物与制药工程学院,江苏南京211816

出　　处：《含能材料》2024年第5期537-544,共8页Chinese Journal of Energetic Materials

摘　　要：为发展绿色无毒、操作简单且结果准确的NC含氮量测量方法,基于硝化纤维素(NC)在碱液中水解后产生的亚硝酸根(NO_(2)^(-))与硝酸根(NO_(3)^(-))的摩尔比与NC含氮量之间的线性关系,采用紫外分光光度计法分析了NC含氮量。在相同的反应条件下水解5种已知含氮量的NC标品,通过紫外分光光度计测定了水解液中的NO_(2)^(-)和NO_(3)^(-)含量,对测量体系的反应条件进行了优化;通过最小二乘法确定NO_(2)^(-)和NO_(3)^(-)的摩尔比(y)与NC标品含氮量(x)之间的线性关系;最后用3种验证用NC样品对此法进行验证。结果表明,通过紫外分光光度计可同时测定碱解液中NO_(2)^(-)和NO_(3)^(-)的含量,其最佳反应条件为:氨基磺酸浓度为20 g·L^(-1),反应时间为30 min;在最佳反应条件下得到了R2为0.9893的y与x间的线性关系式;验证结果表明,采用紫外分光光度计法得到的含氮量与实际含氮量非常吻合,相对标准偏差RSD(n=4)均小于0.150%。A green non-toxic,easy and accuracy analysis method of the nitrogen content in nitrocellulose(NC)was investigated by using ultraviolet spectrophotometer,which was based on a linear relationship between the nitrogen content of NC and the molar ratio of nitrite-to-nitrate ions released after alkaline hydrolysis.Under the same reaction condition,five NC standard samlpes with known nitrogen contents were hydrolyzed.The concentrations of NO_(2)^(-) and NO_(3)^(-) in the hydrolysate were measured by the ultraviolet spectrophotometer,and the reaction condition of measuring system was optimized.The linear relationship be-tween the nitrogen content of NC standards(x)and the molar ratio of nitrite-to-nitrate ions(y)was determined by the least squares method.Finally,three NC samples were used to evaluate the proposed method.Results show that the concentration of NO_(2)^(-) and NO_(3)^(-) in alkaline hydrolysate can be measured simultaneously by ultraviolet spectrophotometer,and the most suitable reaction condition is as follows:the concentration of sulfamic acid of 20 g·L^(-1),and the process time of 30 min.Under the opti-mal reaction condition,the linear relationship between x and y is obtained,and the R2 is 0.9893.The verification results of NCA,NCB and NCC reveal that the nitrogen content determined by ultraviolet spectrophotometer and actual nitrogen contents are in good agreement.The relative standard deviation(n=4)values are all less than 0.150%.

关 键 词：硝化纤维素(NC) 含氮量 紫外分光光度计 NO_(2)^(-)和NO_(3)^(-)测定 

分 类 号：TJ55[兵器科学与技术—军事化学与烟火技术] O657.32[理学—分析化学]