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紫外分光光度计法测定硝化纤维素含氮量OA北大核心CSTPCD

Determination of Nitrogen Content of Nitrocellulose by Ultraviolet Spectrophotometer

中文摘要英文摘要

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(NO2-)与硝酸根(NO3-)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NO2-和NO3-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NO2-和NO3-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NO2-和NO3-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 NO2-and NO3-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 NO2-and NO3-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%.

薛会会;黄娟;张阿磊;陈可泉;周杰;丁亚军;肖忠良

南京理工大学化学与化工学院,江苏 南京 210094||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南京工业大学生物与制药工程学院,江苏 南京 211816

武器工业

硝化纤维素(NC)含氮量紫外分光光度计NO2-和NO3-测定

nitrocellulose(NC)nitrogen contentultraviolet spectrophotometerdetermination of NO2- and NO3-

《含能材料》 2024 (005)

537-544 / 8

10.11943/CJEM2023203

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