中红外漫反射光谱法测定CL-20晶型含量

Quantitative Determination of CL-20 Polymorphs by Mid-infrared Diffuse Reflectance Spectroscopy

采用中红外漫反射光谱技术结合化学计量学偏最小二乘法(PLS)建立了ε-CL-20产品中α-CL-20、γ-CL-20、ε-CL-20的定量校正模型,并对模型进行了交互验证和外部验证。结果表明:三种模型具有较高的准确度和精密度,交互验证决定系数(R2)分别为0.9973、0.9714、0.9848,交互验证标准偏差(RMSECV)分别为0.222%、0.650%、0.670%;外部验证预测标准偏差(RMSEP)分别为0.422%、0.813%、1.02%,配对t检验结果表明预测值与真值之间无显著性差异。基于上述模型的晶型定量分析方法适用于ε-CL-20的产品质量检验以及火炸药工艺过程、长贮过程中ε-CL-20的晶型稳定性研究。

The quantitative calibration models of three polymorphs α-CL-20、γ-CL-20、ε-CL-20 in ε-CL-20 product were established by mid-infrared diffuse reflectance spectroscopy combined with partial least squares（ PLS） method of chemometrics,and the cross-validation and external validation to the models were performed. Results show that three models have high accuracy and precision,the determination coefficients of cross-validation（ R^2） are 0. 9973,0. 9714,0. 9848,respectively,and the root mean square error of cross-validation（ RMSECV） are 0. 222%,0. 650%,0. 670%,respectively. In the external validation,the root mean square error of prediction（ RMSEP） are 0. 422%,0. 813%,1. 02%,respectively,and the paired t-test results show that there is no significant difference between predicted values and actual ones. The quantitative analysis method of CL-20 polymorphs based on the above models can be applied to the product quality test of ε-CL-20,and the studies on the polymorph stability of ε-CL-20 in technical process and long-time storage of explosives and propellants.