建立了同时测定某混合炸药中RDX与FOX-7组分含量的高效液相色谱法.优化后的色谱条件:采用C18色谱柱(150 mm×4.6 mm,5μm),检测波长为210 nm,流动相为乙腈-水(60:40),柱温为25℃,流量为1.0 mL/min,进样体积为2μL.RDX的质量浓度在0.12～0.72 mg/mL范围内与色谱峰面积线性关系良好,相关系数为0.9999,FOX-7的质量浓度在0.24～1.44 mg/mL范围内与色谱峰面积线性关系良好,相关系数为0.9980.RDX、FOX-7的平均回收率分别为99.5％和100.5％,相对标准偏差分别为0.490％和0.258％(n=6).该方法可应用于实际组分检测中.

为了降低RDX的感度,采用溶剂-非溶剂法制备了FOX-7/RDX复合炸药;采用扫描电镜(SEM)分析了FOX-7/RDX复合炸药的微观形貌;采用红外、X射线衍射(XRD)表征了其结构;测试了其撞击感度;采用DSC和TG分析了FOX-7/RDX复合炸药的热性能.结果表明,FOX-7/RDX复合炸药并未形成共晶化合物,而是FOX-7包覆在RDX表面形成的一种复合物;随着FOX-7含量的逐渐增加,RDX晶体包覆得更加完整,FOX-7/RDX复合炸药的撞击感度也逐渐降低;当FOX-7与RDX的质量比为3:1时,其撞击感度由单质RDX的80％ 降为32％.FOX-7/RDX复合炸药的分解放热峰温为232.8℃,较RDX降低了5.2℃,这表明FOX-7/RDX复合炸药的热性能较单质RDX略有降低.

Nitrogen content in nitrocellulose was determined by self-developed fully automatic nitrogen determination analyzer.The effects of sample pretreatment conditions and experimental parameters of fully automatic nitrogen determination analyzer on the results were studied.The accuracy and repeatability of test were discussed.Comparison of fully automatic nitrogen determination analyzer method and traditional alloy reduction method was performed.The results show that the sample pretreatment is carried out by graphite oven heating and temperature gradient mode of saponification, the optimum experimental parameters are determined as steam volume fraction of 80%, preheating time of 30s, reduction reaction time of 7min, boric acid solution volume of 35mL, distillation time of 8 min, indicating that the method of nitrogen content in nitrocellulose detected by fully automatic nitrogen determination analyzer is easy to operate with less time,and can ensure the precision and accuracy of the results.

Uncertainty of determination of copper in some propellant was evaluated.The uncertainty components including sample weighing,sample solution volume,the curve intends to match,measurement repeatability were analyzed and quantified.The combined uncertainty was calculated.The expanded uncertainty of measurement was 0.08%(k=2) as the copper mass fraction was 0.96%.

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.

The accelerated aging tests of high energy nitramine propellants,trietheleneglycol dinitrate(TEGN) propellants and nitroguanidine propellants at various temperatures(95,85,75 and 65 ℃) were carried out.The contents of the effective stabilizer in propellants for various accelerated aging times were measured.The kinetic parameters Ea and lnA of effective stabilizer consumption reaction and the probable mechanism functions g(α) were obtained.Results show that the stabilizer consumption reaction in high energy gun propellants can be described preferably by g(α)=-ln(1-α).The regressive correlation coefficients are more than 0.98.The confidence limits are more than 95%.The apparent activation energies of the effective stabilizer consumption reaction are between 110 kJ·mol-1 and 160 kJ·mol-1.Activation energies of high energy nitramine propellants are more than that of TEGN propellants.Activation energies of nitroguanidine propellants are between the other two propellants.

Electrode potential titration in non-aqueous solvent was used to determine the content of hexahydro1,3,5trinitroStriazine(RDX) and hexahydro1,3,5,7tetranitroStetrazine(HMX). The titration end-point was indicated by the electrode potential curve.The sources of uncertainty in determination and standardization were analyzed and calculated for RDX and HMX. RDX content was (99.710±0.188)%, and HMX content was (99.703±0.189)%.

Dioscorea zingiberensis was refluxed with dil.H2SO4 to liberate diosgenin from the sample,and after neutralization with dil.NaOH solution,the sample solution together with the insoluble residue was extracted with methanol as solvent using the ASE200 Extractor.The methanol extract was diluted to 50 mL with methanol in a volumetric flask and a 10 μL aliquot was taken for HPLC determination.Chromatographic separation was carried out on the YWG C18 column using methanol-H2O(95+5) as mobile phase.UV-detection at the wavelength of 210 nm was adopted in the determination with external standard method.Linearity range of the method was from 0.01 to 2.93 g·L-1,with detection limit of 0.2 mg·L-1.Values of recovery of this method were found in the range of 97.1%-99.8%,and values of RSD′s(n=7) obtain from the results of analysis of 4 substantial samples were in the range of 1.1%-1.5%.

目的:研究并拟定硝酸甘油口服缓释片的处方及制备工艺.方法:将缓释材料压制成片,其外包裹十六醇.采用分光光度法测定含量和释放度,建立两条在不同释放液中测定释放度的工作曲线,r分别为0.997 0,0.998 6,回收率分别为106.5%,95.2%.结果:制备的硝酸甘油口服缓释制剂释放度与文献报道的国外同类产品相近.结论:硝酸甘油口服缓释制剂的处方及制备工艺简单可行.

用气相色谱法检测液晶单体和混晶方便快捷,但在操作中发现有些单体有热降解现象,分子量越小这种现象越明显,通过降低进样口温度可避免这一现象的发生.但分析混晶时,由于不能过多降低进样口温度,必然会导致某些单体的降解,所以在色谱图上出现的小分子杂质不一定是液晶单体或混晶含量不合格,有时是热降解造成的.

The sample is fore treated by HClO_4,then the contents of Pb salt,Cu salt and Al are differently detected by using continuous EDTA titration,which is included direct titration,return titration and substitutive titration.The average recovery is differently 99.95 %(n=7),99.78 %(n=7),100.19 %(n=7),RSD is differently 1.82%,1.32%,1.74%.

In order to study the influence of pH on stability of Iodophor disinfectant,heat acceleration test and chemical measurement method were used to observe the stability of Iodophor disinfectant solution with different pH values.Results: The Iodophor solution containing available iodine 5 g/L was relatively stable at pH 5 and was unstable at pH 8.Conclusion: Acid condition is beneficial to maintenance of stability of iodophor solution.

采用十八烷基非极性键合固定相色谱柱,以甲醇、水、乙酸为流动相,在流速1.0 ml/min,检测波长252 nm,柱温为室温的条件下测定FOX-7的纯度.结果表明,FOX-7与可能的副产物有很好的分离(分离度分别为1.04和1.96),当浓度为6.6～66 μg/ml时,色谱峰高(H)与FOX-7浓度(C)呈线性关系:H=1.5047C+0.7857,相关系数为r=0.9998;采用校正因子归一化法,测得 FOX-7样品纯度为99.70%,RSD为0.22%(n=3).