Processing method of calorimetric curve baseline displacement during thermal analysis of propellant and explosive samples

Abstract

The invention discloses a method for processing the base line displacement of the calorimetric curve during the thermal analysis of propellant and explosive samples. The method for processing the baseline displacement of the thermal analysis calorimetry curve disclosed by the present invention has the following steps: Step 1, obtain and record the thermal decomposition calorimetry curve of the propellant sample according to the microcalorimetry method; Step 2, obtain the specific heat capacity of the sample according to the experimental conditions; The third step is to obtain the mass loss rate of the propellant and explosive with a small sample size; the fourth step is to calculate the heat flow difference caused by the mass loss sample during the thermal decomposition process; the fifth step is to eliminate the baseline displacement of the calorimetric curve of the propellant and explosive sample. This method aims at the baseline displacement problem of the thermal decomposition calorimetry curve of the microcalorimetry method, and provides a processing method for the baseline displacement from the calorimetric principle, which improves the accuracy of the decomposition heat test, and does not affect or change the thermal analysis characteristics. Raw data on peak temperatures can also improve the accuracy of kinetic parameters obtained from calorimetric curves due to the elimination of baseline shifts.

Description

technical field [0001] The invention belongs to the technical field of propellants and explosives, and mainly relates to a method for processing the baseline displacement of the calorimetric curve in the process of thermal analysis of propellant and explosive samples, in particular to the thermal analysis calorimetric curve caused by the change of the system state before and after thermal decomposition of the propellant and explosive sample after thermal decomposition. The processing method for the resulting baseline shift. Background technique [0002] In the process of thermal analysis of explosive samples, it is usually necessary to obtain parameters such as the heat release and thermal decomposition kinetics of the sample. At present, differential scanning calorimetry and microcalorimetry are mainly used to study the heat release of explosive samples, and thermogravimetric analysis is used. Thermal decomposition kinetics of propellant and explosive samples were studied b...

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Problems solved by technology

[0004] This baseline shift often appears in the calorimetric curve of the microcalorimetry method, which shows that the baselines before and after the calorimetric curve are not on the same horizontal line. The large error brings difficulties to the accurate and precise measurement of the heat of decomposition; secondly, because the baseline before and after the calorimetric curve is not on the same level, when using the calorimetric curve for kinetic research, it will affect the shape of the kinetic curve of the conversion rate , thus affecting the accuracy of the kinetic parameters obtained

[0005] At present, for calorimetric curves with baseline displacement, general thermal analysis software provides correction functions such as tilt correction. Tilt correction is generally applicable to the case where the entire calorimetric curve is completely tilted, because it will cause thermal decomposition while correcting the baseline. The change of the peak temperature will modify the original characteristic value. Therefore, for the baseline shift of the system state change before and after the pyrolysis of the propellant sample, the tilt correction is not an appropriate method.

At the same time, for the integration of the calorimetric curve, the general software provides a variety of different integration methods, but due to the inconsistency of the baseline before and after, the selection of different integration methods will bring different calorie value results, resulting in a large experimental error. Still can't fundamentally solve the problems caused by baseline displacement

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