Solution and gas phase deuterium derivatization reactions for gas chromatography/microwave emission detection

Hagen, D.F.; Haddad, Louis C.; Marhevka, John S.

doi:10.1016/0584-8547(87)80067-8

Cited by 12 publications

(1 citation statement)

References 8 publications

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“…16,17 Initially, we tried to prepare di-deuterium analogue, at the benzylic position, of derivative 6. The synthesis of the di-deuterium chloride 3 was attempted by trying to exchange the "acidic" benzylic-protons using a biphasic system NaOD-D 2 O/ CDCl 3 at different temperatures (room temperature to reflux for 24 h) (as shown in Scheme 1).…”

Section: Resultsmentioning

confidence: 99%

Mass spectrometry of 1,2,5-oxadiazole N-oxide derivatives: use of deuterated analogues in fragmentation pattern studies

Cerecetto¹,

González²,

Seoane³

et al. 2004

J. Braz. Chem. Soc.

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Reportamos neste trabalho o estudo sistemático de fragmentação dos derivados de N-óxidos de 1,2,5-oxadiazóis por espectroscopia de massa, usando análogos marcados com deutério para identificar algumas fragmentações críticas. Foi confirmada a perda neutra de CH 2 O a partir do N 2 -óxido de 3-hidroximetil-4-fenil-1,2,5-oxidiazol, usando o análogo mono-deuterado. A perda de OH, a partir do oxigênio do N-óxido, por um rearranjo β-H e δ-H, foi claramente verificada a partir do N 2 -óxido de 3-(4-metilpiperazina-1-metil)-4-fenil-1,2,5-oxidiazol, usando-se o analogo tetra-deuterado adequado. O isômero N-óxido e análogos desoxigenados foram também usados para confirmar a participação do fragmento óxido no processo de defragmentação. This paper reported on the study of fragmentation pattern in mass spectrometry of 1,2,5-oxadiazole N-oxide derivatives involving deuterium-labeled analogues to identify some critical fragmentations. A neutral CH 2 O loss from 3-hydroxymethyl-N 2 -oxide-4-phenyl-1,2,5-oxadiazole was confirmed with the corresponding mono-deuterated analogue. An OH loss, involving the oxygen of N-oxide, via β-H and δ-H rearrangement, was clearly revealed from 3-(4-methylpiperazine-1-ylmethyl)-N 2 -oxide-4-phenyl-1,2,5-oxadiazole using the adequate tetra-deuterated analogue. N-oxide isomer and deoxygenated analogues were also used to confirm the participation of the oxide moiety in the fragmentation process.

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Section: Resultsmentioning

confidence: 99%

Mass spectrometry of 1,2,5-oxadiazole N-oxide derivatives: use of deuterated analogues in fragmentation pattern studies

Cerecetto¹,

González²,

Seoane³

et al. 2004

J. Braz. Chem. Soc.

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Microwave‐Induced Plasma Systems in Atomic Spectroscopy

Broekaert

Engel

2000

Encyclopedia of Analytical Chemistry

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The use of microwave plasmas as radiation sources for optical atomic emission (AES), absorption (AAS) and fluorescence (AFS) spectroscopy and for laser ionization spectroscopy is treated and reference is also made to the use of microwave‐induced plasmas (MIPs) as ion sources for mass spectrometry (MS). Devices for producing both single‐electrode and electrodeless microwave plasmas are treated, in addition to methods for their diagnostics, and results for the analytically relevant plasma parameters are presented. Methods for sample introduction are discussed. They include dry aerosol generation techniques (hydride generation (HG), electrothermal evaporation, spark and laser ablation (LA)) and possibilities for the uptake of wet aerosols. Special reference is made to coupling with gas chromatography (GC) and also to the potential for coupling with high‐performance liquid chromatography (HPLC) Further, the use of microwave plasmas for cross‐excitation in the case of glow discharges (GDs) is treated. The analytical figures of merit in the case of AES with low‐power microwave plasmas, single‐electrode microwave plasmas, plasma torch sources and stabilized capacitively coupled plasmas are given also in the case of atomic absorption, fluorescence and laser ionization with these sources. The developments in MS in the case of both low‐power and high‐power microwave plasmas and in the case of various types of sample introduction are discussed. Applications of MIP atomic spectroscopy are in the fields of biological samples with special reference to microanalysis, and of environmental samples with special emphasis on metal speciation, on‐line monitoring and direct solids analysis. A critical comparison of the methodology with other methods for the determination of the elements and their species is given.

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Microwave Plasma Systems in Optical and Mass Spectroscopy

Jankowski

Reszke²,

Broekaert

et al. 2011

Encyclopedia of Analytical Chemistry

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The art and science of microwave plasma (MWP) optical and mass spectroscopy is briefly presented including very recent advances in the field up to 2011. The use of MWPs as radiation sources for optical emission spectroscopy (OES) and atomic fluorescence spectroscopy (AFS) and as atom reservoirs for atomic absorption spectroscopy (AAS), cavity ringdown spectroscopy (CRDS), and laser‐enhanced ionization spectroscopy (LEIS) as well as ion sources for mass spectrometry (MS) is treated. Devices for producing both E‐type capacitively coupled microwave plasma (CMP)‐electrode and microwave‐induced plasma (MIP)‐electrodeless MWPs, including inductively coupled plasma (ICP)‐like H‐type plasmas, are classified and discussed, in addition to methods of their diagnostics, and results for the analytically relevant plasma parameters are presented. The means of generation of symmetrical plasmas and uses of microplasma devices are also presented with an effort to comment on general classification of microwave (MW) cavities. Further, the use of MWs for boosting of glow discharges (GDs) is treated along with other tandem sources. Methods for the introduction of gaseous, liquid, and solid samples into the MWP are discussed. They include direct vapor sampling (DVS), chemical vapor generation (CVG), and hydride generation (HG) techniques; dry aerosol generation techniques (electrothermal vaporization (ETV); spark ablation (SA); laser ablation (LA); and continuous powder introduction (CPI) as well as wet aerosol generation techniques using both solution and slurry nebulization. Special reference is made to coupling with gas chromatography (GC) and also with various separation techniques for liquids including high‐performance liquid chromatography (HPLC). The analytical figures of merit in the case of OES with low‐power and high‐power MIP, CMP, microwave plasma torch (MPT), MWP‐electrode sources including rotating field sustained plasma and H‐type MWP as well as microplasmas are given. There are also described cases of atomic absorption, fluorescence, and laser ionization with these sources. The developments in MS in the case of both low‐power and high‐power MWPs and in the case of various types of sample introduction techniques are discussed. Applications of MWP analytical spectroscopy are in the fields of biological samples with special reference to microanalysis, and of environmental and industrial samples with special emphasis on element speciation, on‐line monitoring, particle sizing, and direct solids analysis. A critical comparison of the methodology with other spectroscopic methods for the determination of the elements and their species is given.

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Solution and gas phase deuterium derivatization reactions for gas chromatography/microwave emission detection

Cited by 12 publications

References 8 publications

Mass spectrometry of 1,2,5-oxadiazole N-oxide derivatives: use of deuterated analogues in fragmentation pattern studies

Mass spectrometry of 1,2,5-oxadiazole N-oxide derivatives: use of deuterated analogues in fragmentation pattern studies

Microwave‐Induced Plasma Systems in Atomic Spectroscopy

Microwave Plasma Systems in Optical and Mass Spectroscopy

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