顶空固相微萃取-气相色谱法测定N,N-二甲基羟胺

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。...

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Published in核化学与放射化学 Vol. 37; no. 6; pp. 441 - 446
Main Author 王玮 吴继宗 邓惟勤 陶苗苗 谈树苹
Format Journal Article
LanguageChinese
Published 中国原子能科学研究院 放射化学研究所,北京,102413 2015
Subjects
N,N-二甲基羟胺
气相色谱法
顶空固相微萃取
气相色谱法
顶空固相微萃取
gas chro-matography
N,N-dimethylhydroxylamine
N ,N-二甲基羟胺
headspace solid-phase micro-extraction
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Summary: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。
Bibliography: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.
11-2045/TL
N,N-dimethylhydroxylamine headspace solid-phase micro-extraction; gas chro-matography
WANG Wei, WU Ji-zong, DENG Wei-qin, TAO Miao-rniao, TAN Shu-ping（ China Institute of Atomic Energy, P. O. Box 275（88）, Beijing 102413, China）
ISSN:0253-9950
DOI:10.7538/hhx.2015.37.06.0441