贾林, 张皋, 胡玲, 刘红妮, 杨彩宁, 王景荣. ASE-HPLC检测某型号球形发射药中的叠氮硝胺、硝化甘油、Ⅱ号中定剂含量的研究[J]. 分析测试技术与仪器, 2008, 14(4): 222-225.
引用本文: 贾林, 张皋, 胡玲, 刘红妮, 杨彩宁, 王景荣. ASE-HPLC检测某型号球形发射药中的叠氮硝胺、硝化甘油、Ⅱ号中定剂含量的研究[J]. 分析测试技术与仪器, 2008, 14(4): 222-225.
JIA Lin, ZHANG Gao, HU Ling, LIU Hong-ni, YANG Cai-ning, WANG Jing-rong. Determination of the Components in the Globule Gun-propellantUsing Accelerated Solvent Extraction(ASE) Followed by HPLC[J]. Analysis and Testing Technology and Instruments, 2008, 14(4): 222-225.
Citation: JIA Lin, ZHANG Gao, HU Ling, LIU Hong-ni, YANG Cai-ning, WANG Jing-rong. Determination of the Components in the Globule Gun-propellantUsing Accelerated Solvent Extraction(ASE) Followed by HPLC[J]. Analysis and Testing Technology and Instruments, 2008, 14(4): 222-225.

ASE-HPLC检测某型号球形发射药中的叠氮硝胺、硝化甘油、Ⅱ号中定剂含量的研究

Determination of the Components in the Globule Gun-propellantUsing Accelerated Solvent Extraction(ASE) Followed by HPLC

  • 摘要: 采用快速溶剂萃取(ASE)技术和高效液相色谱法测定某球形药中叠氮硝胺(DIANP)、硝化甘油(NG)和II号中定剂(C2)的含量.ASE提取条件:二氯甲烷做萃取溶剂,萃取温度100 ℃,静态萃取10 min,萃取2次. HPLC测定条件:YWG C18柱(150×4.6 mm,10 μm),以甲醇和水作为流动相,梯度洗脱,流速1 mL/min,检测波长210 nm. 测定结果表明DIANP、NG、C2平均回收率分别为99.6%、100.3%、99.4%,RSD分别为0.7%、0.8%、0.9%(n=5),检出限分别为2.1、1.5和0.2 mg/L,线性范围分别为0.02~0.98 g/L, 0.03~1.38 g/L, 0.002~0.124 g/L.用此方法共检测某批球形发射药样品5份,检测结果与滴析-HPLC法检测结果相当.

     

    Abstract: 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.

     

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