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

中文关键词:  发射药,快速溶剂萃取(ASE),高效液相色谱

英文关键词:gun-propellant,Accelerated Solvent Extraction (ASE),HPLC

中文摘要:

      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.

英文摘要:

      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.