后化学发光法检测水中微量偏二甲肼

Determination of Trace Unsymmetrical Dimethyl Hydrazine in Water by Luminol-Potassium Periodate Post-chemiluminescence Method

基于偏二甲肼在高碘酸钾-鲁米诺化学发光反应体系中产生后化学发光反应,建立了后化学发光反应测定水中微量偏二甲肼的新方法。系统研究了该体系的影响因素,实验结果表明,最佳发光条件为:负高压为-800 V,管长为60 cm,NaOH浓度为0.1 mol.L-1,鲁米诺的浓度为1.0×10-5mol.L-1,高碘酸钾浓度为2.0×10-5mol.L-1,测定的线性范围为1.0×10-6～1.0×10-4g.L-1,检出限为3.3×10-7g.L-1。对4.0×10-6g.L-1的偏二甲肼进行11次平行测定的相对标准偏差为2.7%。该法用于模拟水样的测定,并对该发光反应的发光机理进行了初步探讨。

A post chemiluminescence（PCL） phenomenon was observed when unsymmetrical dimethyl hydrazine（UDMH） solution was injected into a solution after the finish of CL reaction of alkaline luminol and potassium periodate. A new method for the determination of trace UDMH was established based on the studies of the CL reaction conditions including the concentration of potassium periodate and luminol,the length of tube,the velocity of solution flow,the luminal alkalinity（NaOH） and other experiments. The linear response range of this method was from 1.0 ×10-6to 1.0 ×10-4g·L-1 with a detection limit of 3.3×10-7g·L-1. The relative standard deviation for 4.0 ×10-6g·L-1 UDMH solution was 2.7% for 11 tests. This method has been used to determine UDMH in water with satisfactory results. The PCL mechanism is also discussed briefly.