偏二甲肼废水中亚硝基二甲胺的高效液相色谱测定法

目的建立高效液相色谱法测定亚硝基二甲胺的方法。方法采用反相高效液相色谱法测定火箭推进剂偏二甲肼废水中亚硝基二甲胺的含量。色谱条件:色谱柱CNWSIL-C18(4.6×250 mm,5μm),流动相甲醇∶水为15∶85,流速为1.0ml/min,柱温28℃,紫外检测器检测波长为230 nm。结果亚硝基二甲胺在10～500μg/L范围内线性关系良好(r2=0.999 9);高、中、低3种浓度加标平均回收率分别为104.1%、96.93%、92.5%(RSD分别为1.6%、1.8%、1.7%),高、中、低3种浓度精密度RSD为0.13%、0.75%、0.47%,最低检测限为0.5μg/L。结论该方法准确,快速,可用于亚硝基二甲胺的测定。

Determination of N-nitrosodimethylamine in unsymmetrical dimethylhydrazine wastewater by high performance liquid chromatography

[Objective]To establish a method for determination of N-nitrosodimethylamine by high performance liquid chromatography.[Methods]Reversed-phase high performance liquid chromatography(RP-HPLC) was applied for determination of N-nitrosodimethylamine in unsymmetrical dimethylhydrazine wastewater of rocket propellant.Chromatographic conditions: CNWSIL C18 column(4.6×250 mm,5 μm) was adopted,the mobile phase was methanol and water(15∶ 85),the flow rate was 1.0 ml/min,the column temperature was 28 ℃,and the detection wavelength was 230 nm.[Results]There was a good linear relation in the range of 10-500 μg/L of N-nitrosodimethylamine(r=0.999 9).The average recovery of standard addition of upper,middle and lower concentration group was respectively 104.1%、96.93% and 92.5%(RSD was respectively 1.6%,1.8% and 1.7%).The precision RSD of upper,middle and lower concentration group was 0.13%,0.75% and 0.47%,respectively.The lowest detection limit was 0.5 μg/L.[Conclusion]This method is accurate and rapid,and it can be used to determine the N-nitrosodimethylamine.