针对硝化甘油生产过程中硝化酸检测存在安全隐患和检测时间长的问题,采用近红外光谱技术研究了硝化酸的快速检测方法,建立了硫酸、硝酸和硝化甘油组分的定量模型并进行了应用验证,并与化学分析法进行了对比.结果 表明,所建模型的交互验证决定系数(R2)分别为0.966 6、0.958 5和0.9791,交互验证的均方根误差(RMSECV)分别为0.195％、0.329％和0.064％,外部验证的均方根误差(RMSEP)分别为0.271％、0.388％和0.121％.显著性检验(t(H2SO4)=0.59,t(HNO3)=1.64,t(NG)=1.59)表明,在显著水平为0.05时,近红外光谱法与化学分析法无显著差异.每个样品的检测时间统计不超过2 min.表明该方法快速、准确,能够满足硝化甘油在线质量检测和自动化生产的要求.

The gun-powder sample was treated by solid-liquid extraction method,the components in unknown gun-powder were anatomized by gas chromatograph-mass spectrometry.Selective ion quantitative method was used for quantitative analysis.The concentration of target compound was linear with chromatographic peak area in the range of 20-50?mg/L,the correlation coefficient was 0.994?0-0.999?6.The recovery rate was 96.9%-104.3% and relative standard deviation of analysis results was 0.4%-4.9%(n=5).Gas chromatograph-mass spectrometry is suitable for the analysis of gun-powder anatomy research.

In alkali high temperature conditions,by using the degradation seperation method from high-molecular compound,analyzing Fourier transform infrared spectrogram and spectrogram of GC-MS spectrometer for each composition,high polymer composition and assistant composition of unknown matter were identified and the unknown adhesive composition was confirmed.