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用反相高效液相色谱法分析单基火药中的二苯胺和光电二极管阵列检测器对二苯胺变化规律的探讨

Analysis of Diphenylamine in the Single-Base Propellant by the Method of Reversed-Phase HPLC and study of Variable Rules for Diphenylamine by the Photodiode Array Detector

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【作者】 毕汝麒高峰刘向文邓巍

【Author】 Bi Ruqi, Gao Feng, (Shenyang Institute of Chemical Technology) Liu Xianwen, Deng Wei (The Chinese People’s Liberation Army 81886)

【机构】 沈阳化工学院沈阳化工学院中国人民解放军81886部队

【摘要】 本文叙述了用反相高效液相色谱法分离分析9/(单基火药中的安定剂二苯胺,以Zorbax DOS柱,甲醇/水(95:5V/V)为流动相,用光电二极管阵列检测器,检出二苯胺和分解产物的光谱一色谱三维图进行定性,并观察单基火药随存放过程的增长而变化的情况,用SPD—2AS,UV检测器和C—R 2AX微处理机,外标法定量,标准偏差为7.5×10-3,2.2×10-2,相对误差为-0.47%,变异系数为0.52,1.79,回收率可达99.62%,由分析结果可见本法的准确度和精密度,均令人满意,分析时间可缩短至几分钟。

【Abstract】 In this paper a methol of separating analysis of diphenylamine stabilizer in single-base propellant 9/7 by the reversed-phase high performance liquid chromatography is described, The chromatographic conditions were: the stationary phase: Zorbax ODS column; the mobile phase: CH3OH/H2O(90/10 V/V); the detector: photodiode array detector. The detected three dimensional spectro-chromatograms of the diphenylamine stabilizer and the decomposed product were observed and analysed qualitatively. The quantitative analysis has performed by the external standard for the SPD-2AS UV detector and the CR—2Axmicroprocessor. The results were as follows: the standard deviation, 7.5×10-3 relation, -0.47%; variable coefficient, 0.52; recovery 99.6%. It could be observed from the results of quantitative analysis and the three dimensional spectro-chromatograms that diphenylamine has decreased gradually and the decomposing product has increased as the time of store has prolonged. The time of analy-sis may be shortened to several minutes and the disturbance of determination by the decomposing product from volumetric bromide method has been overcome.

  • 【文献出处】 沈阳化工学院学报 ,Journal of Shenyang Institute of Chemical Technology , 编辑部邮箱 ,1987年01期
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