DAP-4 (C6N2H14) (NH4) (ClO4)3 has been synthesized recently as an ammonium perchlorate-based molecular perovskite energetic material with higher stability and outstanding performances. In this study, rapid thermal cracking infrared spectroscopy is applied to study the thermal pyrolysis properties and combustion process of DAP-4. Under different temperatures and pressure with a heating rate of 1000 degrees C center dot s- 1, the gaseous products in the rapid pyrolysis process are mainly CO, CO2, H2CO, HCN, and HCl. Above 700oC, the pressure affects the ratio of the gas products, but the temperature does not. Based on the relative ratio of the different gas products, a thermal pyrolysis mechanism was proposed. The heat of explosion (Delta Hdet), enthalpy of combustion(Delta cH theta), and standard enthalpies of formation (Delta fH theta) are determined to be -2527.39 kJ center dot mol-1, -2492.06 kJ center dot mol-1 and -483.96 kJ center dot mol-1, respectively. The self-catalytic heating time is 99.5 min, the temperature at the initial detection point is 280.1 degrees C, and the maximum temperature rise rate is 49.1 degrees C center dot min- 1. The thermal safety experimental results showed that DAP-4 has a relatively good security performance. This study provides new insight into the mechanism of pyrolysis of DAP-4 as a potential energetic material.

以某改性单基发射药为研究对象,采用聚焦微波消解法,将试样消解为试样溶液,以火焰原子吸收法测定其中的钾元素含量,结果表明,钾元素的平均回收率为104.3％(n=7),相对标准偏差(RSD)为3.47％(n=7),其测定结果与传统电热板消解法无显著性差异,消解时间缩短1h.

通过卤素水分测定仪和烘箱法测定了硝化棉的水分含量,研究了影响卤素水分测定仪测定硝化棉水分含量的因素,并与传统烘箱法进行了对比.结果表明,干燥温度、干燥时间对卤素水分测定仪测定硝化棉水分含量影响较小,样品质量、质量损失率是影响卤素水分测定仪测定硝化棉水分的重要因素;卤素水分测定仪测试结果与烘箱法结果基本一致,测量结果重复性好,试验相对标准偏差小,极大的缩短了检测时间,可以用于实际生产中的质量控制.

The method was established for determining the components of organic impurity without the self-reference material(RM) by GC–FID.The signal of GC–FID was caliberated with the compound whose structure was similar with the organic impurity to be determined,and after the mass response(Si) of GC–FID of the impurity counted by ECN,the components of impurity in sample were determined.DBS purity RM as the example,the sum of organic impurities in DBS RM was(0.29±0.07)%(k=2).The major sources of uncertainty of measurement were Si and the repeatability.

The method for determining the components in a energetic azid wastewater was established.DIANP was determinated by HPLC with UV detection.The HPLC separation was performed on a YWG C18 column(150 mm×4.6 mm,10 μm) with methanol and water as the mobile phase at a flow rate of 1.0 mL/min.The detection wavelength were 230 nm.The spectrophotometer conditions were as follows:FeCl3 solution,pH 2~3,the detection wavelength were 460 nm.The recovery of DIANP was 97.8%～100.9% with a RSD of 1.2%(n=5),the limits of detection was 1.5 mg/L,the linear range was 17～859 mg/L.The recovery of DMSO was 98.2%～101.9% with a RSD of 1.5%(n=5).The recovery of NaN3 was 98.9%～100.5% with a RSD of 0.6%(n=5),the limits of detection was 1.5 mg/L,the linear range was 5.7～57.0 mg/L,the apparent absorptivity was 901 L/(mol·cm) at 460 nm.The method was applied to actual samples.

In order to certificate the standard substance 1,5-diazido-3-nitrazpentane(DIANP),an electrode potential titration of determining the purity of DIANP was established.The conditions of the titration method were as follow:dimethysulfoxide(DMSO)as solvent,adding sodium hydroxide solution as reaction regent,and making N-3 in DIANP and Ag+ in AgNO3 react to form the precipitate of AgN3.The purity of standard substance DIANP calculated by the EQP curve was 99.85% and the relative standard derivation was 0.13%.There was no significant varation between the results obtained by electrode potential titration and HPLC method.The expanded uncertainty of this method was 0.3%.

A novel method for determination of the nitrogen content in nitrocellulose was established using a polarized light microscope.Senarmont method was used to determine the average optical path difference.The results show that the relationship(w=-0.0466λ+12.388) between the nitrogen content and the optical path difference was linear with a correlation coefficient of 0.9993 when the range of the nitrogen content in nitrocellulose were 11.0%-13.8%.Certified nitrocellulose reference materials were used to evaluate the method and the results show that the recoveries ranged from 99.7% to 100.2% with the relative standard deviations falling between 0.15% and 0.20%.The method is simple,accurate and environment-friendly.

Objective: to establish the method for determining the components in globule gun-propellant samples.Method: the samples were extracted by ASE200 and determinated by HPLC with UV detection.Parameters such as solvent,temperature,pressure and time were investigated thoroughly.The ASE conditions were as follows: dichloromethane,100 ℃ and two 10 min cycles were chosen as the extraction solvent,the temperature and time,respectively.The HPLC separation was performed on a YWG C18 column(150×4.6 mm,10 μm) with methanol and water as the mobile phase at a flow rate of 1.0 mL/min.The detection wavelength was 210 nm.Results: the average recovery of DIANP,NG and C2 were 99.6%,100.3% and 99.4%,with a RSD of 0.7%,0.8% and 0.9%(n=5).The limits of detection were 2.1 mg/L、1.5 mg/L、0.2 mg/L,respectively.The linear range were 0.02~0.98 g/L,0.03~1.38 g/L,0.002~0.124 g/L,respectively.The method was applied to one samples for 5 times.

Through the analysis of uncertainty of measurement during measuring FID detectability,the uncertainty of FID detectability was estimated.The combined relative uncertainty of FID detectability was 1.7%,and the expand uncertainty was 3.4%(n=2).The rationality of evaluation result was validated contrastingly.