Gas chromatographic determination of 1,1-dimethylhydrazine in water samples by solid-phase microextraction with derivatization
Abstract1,1-Dimethylhydrazine (1,1-DMH) used as a rocket fuel component is highly reactive and unstable compound. It greatly complicates its accurate and express determination in environmental samples. Goal of this work was to develop a method for its express determination in water samples based on solid-phase microextraction with preliminary derivatization. Acetone was selected as reagent for derivatization because during its reaction with 1,1-DMH, volatile and hydrophobic acetone dimethylhydrazone (ADMH) was formed. It was established that fiber based on 100-micron polydimethylsiloxane provides the most efficient extraction of ADMH from water at extraction time 2 min. Optimal concentration of acetone was 30 mg/mL. The minimum time for reaction of 1,1-DMH with acetone is 10 minutes. Addition of acids and alkali reduced ADMH response that may be caused by degradation of 1,1-DMH and reduction of derivatization rate. Addition of salt allowed to increase the response of ADMH however made impossible the quantitative determination of 1,1-DMH. Dependence of ADMH response on the concentration of 1,1-DMH at optimized parameters is linear in the concentrations range of 0.1-100 mg/L and can be used for quantitative determination of 1,1-DMH in water. Detection limit of the developed method is 0.02 mg/L. Reproducibility index of the method in the whole range of concentrations did not exceed 7%, accuracy index - 15%. Developed method is simple, inexpensive, accurate, automated and can be recommended for implementation in laboratories conducting environmental monitoring in areas of rocket-carriers fall.
1 Kassimov NS, Grebenyuk VB, Koroleva TV, Proskuryakov YV (1994) Pochvovedeniye 9:110-120.
2 Carlsen L, Kenessov BN, Batyrbekova SY (2008) Environmental Health Insights 1:11-20.
3 Kenessov BN (2010) Chemical Bulletin of Kazakh National University 3:403-406. (In Russian) http://dx.doi.org/10.15328/chemb_2010_3403-406
4 Samsonov DP, Bornovalova GV, Pervunina RI, Zhiryukhina NP (1998) J Anal Chem+ 53:169-172.
5 Savchuk SA, Brodskiy YS, Formanovskiy AA, Rudenko BA (1998) J Anal Chem+ 53:668-671
6 Denisov AA, Smolenkov AD, Shpigun OA (2004) J Anal Chem+ 59:452-456. http://dx.doi.org/10.1023/B:JANC.0000026237.44977.04
7 Kenessov BN, Kalugina SM, Alimzhanova MB, Baimatova N, Batyrbekova SY (2007) Chemical Bulletin of Kazakh National University 5:73-77
8 Diekmann J, Biefel C, Rustemeier K (2002) J Chromatogr Sci 40:509-514. http://dx.doi.org/10.1093/chromsci/40.9.509
9 An Z, Li P, Zhang X, Liu L (2014) J Liq Chromatogr R T 37:1212-1225. http://dx.doi.org/10.1080/10826076.2012.745147
10 Smolenkov AD, Krechetov PP, Pirogov AV, Koroleva TV, Bendryshev AA, Shpigun OA, Martynova MM (2005) Int J Environ An Ch 85:1089-1100. http://dx.doi.org/10.1080/03067310500191454
11 Kosyakov DS, Ulyanovskii NV, Bogolitsyn KG, Shpigun OA (2014) Int J Environ An Ch 94:1254-1263. http://dx.doi.org/10.1080/03067319.2014.940342
12 Smolenkov AD, Shpigun OA (2012) Talanta 102:93-100. http://dx.doi.org/10.1016/j.talanta.2012.07.005
13 Pawliszyn J. (1997) Solid phase microextraction: Theory and practice. Wiley-VCH, Inc., USA. ISBN: 0471190349
14 Kenessov BN, Koziel JA, Grotenhuis T, Carlsen L (2010) Anal Chim Acta 674:32-39. http://dx.doi.org/10.1016/j.aca.2010.05.040
15 Kenessov B, Alimzhanova M, Sailaukhanuly Y, Baimatova N, Abilev M, Batyrbekova S, Carlsen L, Tulegenov A, Nauryzbayev M (2012) Sci Total Environ 427:78-85. http://dx.doi.org/10.1016/j.scitotenv.2012.04.017
16 Yergozhin YeYe, Solomin VA, Lyapunov VV, Tsukerman VG (2000) A method for determination of 1,1-dimethylhydrazine [Metod opredeleniya 1,1-dimetilgidrazina]. Preliminary Patent of the Republic of Kazakhstan [Predvaritelnyi patent Respubliki Kazakhstan]. (In Russian)
17 Paramonov SA, Ulyanov AV, Buryak AK (2010) Russ Chem B+ 59:528-532. http://dx.doi.org/10.1007/s11172-010-0141-0
18 Smirnov RS, Smolenkov AD, Bolotnik TA, Shpigun OA (2013) J Anal Chem+ 68:837-844. http://dx.doi.org/10.1134/S1061934813090116
19 Smolenkov AD, Chernobrovkina AV, Smirnov RS, Chernobrovkin MG, Shpigun OA (2013) Int J Environ An Ch 93:1286-1295. http://dx.doi.org/10.1080/03067319.2012.736975
20 Kenessov BN, Sailaukhanuly Y, Koziel J, Carlsen L, Nauryzbayev M (2011) Chromatographia 73:123-128. http://dx.doi.org/10.1007/s10337-010-1820-6
21 RMG 61-2010. Accuracy, trueness and precision measures of the procedures for quantitative chemical analysis. Methods of evaluation [GSI. Pokazateli tochnosti, pravilnosti, pretsizionnosti metodik kolichestvennogo himicheskogo analiza. Metodyi otsenki]. Moscow, Russia, 2012. (In Russian)
This work is licensed under a Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International License.Authors retain copyright and grant the journal right of first publication with the work simultaneously licensed under a Creative Commons Attribution License that allows others to share the work with an acknowledgement of the work's authorship and initial publication in this journal.