气相色谱-质谱法测定大气中偏二甲肼
GC-MS Determination of Unsymmetrical Dimethylhydrazine in Air
摘 要
利用气泡吸收器富集大气中的偏二甲肼气体,以水杨醛与水以体积比1比50混合的溶液作为吸收液,偏二甲肼经水杨醛于50 ℃下衍生化3 h后,供气相色谱-质谱法分析检测.结果表明:当采集流量为0.2 L·min-1时,吸收器对偏二甲肼的吸附效率为95%~98%.偏二甲肼的质量浓度在40.0 mg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)为0.878 mg·L-1.测定结果的相对标准偏差(n=6)为2.96%~4.09%,加标回收率为 88.0%~93.0%.
大气
偏二甲肼
衍生化反应
水杨醛
GC-MS
Air
UDMH
Derivatization reaction
Salicylaldehyde
Abstract
A bubbling absorber was used for the collection and enrichment of unsymmetrical dimethylhydrazine (UDMH) in air with mixed solution of salicylaldehyde and water (1+50) as absorbent.The absorbed analyte in absorbent were derivatized with salicylaldehyde at 50 ℃ for 3 h,and analyzed by GC-MS.It was found that when the sampling flow rate was 0.2 L·min-1,the absorption efficiency of UDMH achieved to 95%-98%.Linear relationship between values of peak area and mass concentration of UDMH was obtained in the range within 40.0 mg·L-1,with detection limit (3S/N) of 0.878 mg·L-1.Tests for precision and recovery were made by standard addition method,giving RSD′s (n=6) in the range of 2.96%-4.09% and values of recovery in the range of 88.0%-93.0%.
中图分类号 O657.63
所属栏目 工作简报
基金项目 总装备部司令部试验技术研究项目(20070116)
收稿日期 2009/7/12
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备注曹晔(1966-),女,山西大同人,副研究员,博士研究生,主要研究方向为液体推进剂检测.
引用该论文: CAO Ye,WANG Li,HAN Zhuo-zhen,ZHANG Guang-you,LIU Jian-guo. GC-MS Determination of Unsymmetrical Dimethylhydrazine in Air[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(10): 1184～1186
曹晔,王力,韩卓珍,张光友,刘建国. 气相色谱-质谱法测定大气中偏二甲肼[J]. 理化检验－化学分册, 2010, 46(10): 1184～1186
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参考文献
【1】MARCEL A R,HANS R B.Determination of daminozide and dimethylhydrazine residues in swiss apple juice concentrates using gas chromatography-mass spectrometry[J].J Agric Food Chem,1991,39:176-181．
【2】STEINBRECHER K,SAXTON W,OEHLER G A.Improved gas chromatographic mehod for determination of daminozide by alkaline hydrolysis and 2-nitrobenzaldehyde derivatization and survey results of damnozide in agricultural products[J].Journal of Association Official Analytical Chemistry,1990,73:12-15．
【3】BRINKMAN J H,WAGENAAR D R,QUIRIJNS J K.Determination of daminozide residues in apples using gas chromatography with nitrogen-phosphorous detection[J].Journal of Chromatography A,1996,723:355-360．
【4】孔祥虹,汤桦,李建华,等.气相色谱-质谱法测定浓缩苹果汁中丁酰肼残留量[J].理化检验-化学分册,2006,42(9):721-725．
【5】张有智,李正莉,忘煊军,等.微量偏二甲肼检测技术研究进展[J].化学推进剂与高分子材料,2008,6(3):20-23．
【6】张光友,曹晔.肼类动态标准气体发生装置的设计[J].上海航天,2003,20(1):53-56．
【2】STEINBRECHER K,SAXTON W,OEHLER G A.Improved gas chromatographic mehod for determination of daminozide by alkaline hydrolysis and 2-nitrobenzaldehyde derivatization and survey results of damnozide in agricultural products[J].Journal of Association Official Analytical Chemistry,1990,73:12-15．
【3】BRINKMAN J H,WAGENAAR D R,QUIRIJNS J K.Determination of daminozide residues in apples using gas chromatography with nitrogen-phosphorous detection[J].Journal of Chromatography A,1996,723:355-360．
【4】孔祥虹,汤桦,李建华,等.气相色谱-质谱法测定浓缩苹果汁中丁酰肼残留量[J].理化检验-化学分册,2006,42(9):721-725．
【5】张有智,李正莉,忘煊军,等.微量偏二甲肼检测技术研究进展[J].化学推进剂与高分子材料,2008,6(3):20-23．
【6】张光友,曹晔.肼类动态标准气体发生装置的设计[J].上海航天,2003,20(1):53-56．
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