叠氮含能化合物生产废水关键组分含量测定研究

摘要

叠氮含能化合物废水用碱中和后,采用高效液相色谱法和分光光度法分别测定其中叠氮含能化合物DIANP、二甲亚砜(DMSO)、NaN3的含量.HPLC测定条件:YWG C18柱(150 mm ×4.6 mm,10μm),以甲醇和水作为流动相,梯度洗脱,流速1 mL/min,检测波长230nm.分光光度法测定条件:显色剂为FeCl<,3>,pH 2～3时显色,检测波长460 nm.结果表明,DIANP回收率为97.8%～100.9%,RSD=1.2%(n=5),检出限为1.5 mg/L,标准曲线的线性回归系数r=0.997 7,线性范围为17～859 mg/L;DMSO回收率98.2%～101.9%,RSD=1.5%(n=5);NaN,回收率98.9%～100.5%,RSD=0.6%(n=5),检出限为1.5 mg/L,标准曲线的线性回归系数r=0.999 1,线性范围为5.7～57.0 mg/L,表观摩尔吸光系数901 L(mol·cm).该方法已经应用于实际生产线废水的检测和治理,效果良好.%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.