顶空固相微萃取-气相色谱法测定N,N-二甲基羟胺

Determination of N,N-Dimethylhydroxylamine by Headspace Solid-Phase Micro-Extraction and Gas Chromatography

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65μm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1.65~49.4mmol/L范围内有良好的线性关系(r=0.997 3),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。

A method for the determination of N, N-dimethylhydroxylamine（DMHAN） has been established by coupling headspace solid-phase micro-extraction （HS-SPME） with gas ehromatography（GC）. The 65 μm PDMS/DVB coating was selected for micro-extractor. The extraction conditions, such as extraction time, extraction temperature, solution acidity, headspaee 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.