顶空固相微萃取-气相色谱法测定<i>N,N</i>-二甲基羟胺

顶空固相微萃取-气相色谱法测定N,N-二甲基羟胺

摘要: 建立了顶空固相微萃取-气相色谱测定-N,N-二甲基羟胺(DMHAN)的分析方法。采用65 μm聚二甲基硅氧烷/二乙烯基苯（PDMS/DVB）进行萃取，考察了萃取时间、萃取温度、溶液pH值、顶空体积及解吸时间等因素的影响，确定了顶空固相微萃取-气相色谱分析DMHAN的最佳实验条件。DMHAN浓度在1.65~49.4 mmol/L范围内有良好的线性关系(r=0.9973)，当浓度为8.24 mmol/L时相对标准偏差为2.1%（n=5），检出限为4.67×10^-2 mmol/L，重加回收率为96.1%~103%。该方法操作简单、稳定，适合后处理料液中DMHAN的测定。

Abstract: A method for the determination of N, N-dimethylhydroxylamine(DMHAN) has been established by coupling headspace solid-phase micro-extraction (HS-SPME) with gas chromatography(GC). The 65 μm PDMS/DVB coating was selected for micro-extractor. The extraction conditions, such as extraction time, extraction temperature, solution acidity, headspace volume and desorption time were discussed and optimized. The linear range of DMHAN was 1.65-49.4 mmol/L (r=0.997 3). The relative standard deviation was 2.1% (n=5). The detection limit is 4.67×10^-2 mmol/L. The recoveries are from 96.1% to 103%. This method is simple, stable and suitable for the determination of DMHAN in the process solution of spent fuel reprocessing.