Micro-Synthesis and Electron Ionization Mass Spectral Analysis of O-Alkyl N,N-Dialkylphosphoramidocyanidates

2005 ◽  
Vol 11 (3) ◽  
pp. 309-318 ◽  
Author(s):  
Arvind. K. Gupta ◽  
Meehir Palit ◽  
Deepak Pardasani ◽  
Purushottam Shakya ◽  
Rajendra K. Srivastava ◽  
...  
Keyword(s):  
Mass Spectra ◽  
Chemical Warfare Agent ◽  
Chemical Warfare ◽  
Toxic Chemicals ◽  
Ionization Mass ◽  
Mass Spectral Analysis ◽  
Mass Spectral ◽  
Ms Analysis ◽  
Chemical Weapons Convention ◽  
Chromatographic Mass

This communication describes the microsynthesis and gas chromatographic/mass spectrometric (GC/MS) analysis of O-alkyl N,N-dialkylphosphoramidocyanidates (ADAPCs), which are analogs of the chemical warfare agent, Tabun. The study was undertaken with a view to develop a spectral database of ADAPCs for verification purposes of the Chemical Weapons Convention (CWC). Reported microsynthetic approaches have advantages over traditional synthesis in terms of efficiency, synthetic waste and exposure to toxic chemicals. GC/MS analysis of a variety of these compounds (ADAPCs) was performed. Based on the obtained mass spectra of structurally diverse ADAPCs, the fragmentation routes are proposed, which explains most of the characteristic ions.

Gas Chromatography Electron Ionization Mass Spectrometric Analysis of O-Alkyl Methylphosphinates for Verification of Chemical Weapons Convention

2009 ◽  
Vol 15 (5) ◽  
pp. 579-585 ◽  
Author(s):  
Deepak Pardasani ◽  
Pankaj K. Kanaujia ◽  
Vijay Tak ◽  
Prabhat Garg ◽  
Avik Mazumder ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Mass Spectra ◽  
Electron Ionization ◽  
Mass Spectrometric ◽  
Chemical Weapons ◽  
Spectrometric Analysis ◽  
Ionization Mass ◽  
Ms Analysis ◽  
Chemical Weapons Convention ◽  
Hydrogen Rearrangement

We describe the gas chromatography/mass spectrometric (GC/MS) analysis of O-alkyl methylphosphinates (AMPs), which are included in Schedule 2B4 chemicals in the Chemical Weapons Convention (CWC). GC/MS analysis of a variety of AMPs and their deuterated analogs revealed that their fragmentations were determined by α-cleavages, McLafferty +1 and hydrogen rearrangement. Based on the obtained electron ionization mass spectra of AMPs, the fragmentation routes were rationalized, which were substantiated by the GC/MS analysis of deuterated analogs.

Rapid, In-Situ Detection of Chemical Warfare Agent Simulants and Hydrolysis Products in Bulk Soils by Low-Cost 3D-Printed Cone Spray Ionization Mass Spectrometry

The Analyst ◽  
2021 ◽  
Author(s):  
Hilary M. Brown ◽  
Trevor J. McDaniel ◽  
Karan R. Doppalapudi ◽  
Christopher C. Mulligan ◽  
Patrick Fedick
Keyword(s):  
Low Cost ◽  
Chemical Warfare Agents ◽  
Chemical Warfare Agent ◽  
Chemical Warfare ◽  
Ionization Mass ◽  
Chemical Weapons Convention ◽  
Warfare Agents ◽  
3D Printed ◽  
In Situ Detection

Chemical warfare agents (CWAs) are toxic chemicals that have been used as disabling or lethal weapons in war, terrorist attacks, and assassinations. The Chemical Weapons Convention (CWC) has prohibited the...

The sonolysis of cytosine and thymine

1987 ◽  
Vol 65 (6) ◽  
pp. 1162-1164 ◽  
Author(s):  
Tain-Jen Yu ◽  
Ronald G. Sutherland ◽  
Ronald E. Verrall
Keyword(s):  
Spectral Analysis ◽  
Degradation Products ◽  
Mass Spectral Analysis ◽  
Mass Spectral ◽  
Ms Analysis ◽  
Alloxan Monohydrate ◽  
Sonolytic Degradation ◽  
Oxaluric Acid ◽  
Chromatographic Mass

Sonolysis of cytosine has been studied at 630 kHz in the presence of air and nitrogen. The degradation products were identified by gas chromatographic – mass spectral analysis. Under aerated conditions the following products were found: urea, formyl urea, parabanic acid, isobarbituric acid, oxaluric acid, alloxan monohydrate, alloxantin, dialuric acid, and uracil glycols. Under nitrogen the degradation products were isobarbituric acid, alloxan monohydrate, and uracil glycols. The observed products have been used to develop a possible mechanism for the sonolytic degradation. There appears to be some similarity with the products reported from radiolysis studies of this compound. Sonolysis of thymine in the presence of air was reinvestigated and the gc–ms analysis shows that a previously reported, unidentified, product may be 5-hydroxy-5-methylbarbituric acid.

scholarly journals Discrimination of structural isomers of amphetamine using carbon dioxide negative-ion chemical ionization mass spectrometry

1997 ◽  
Vol 13 (2) ◽  
pp. 151-161 ◽  
Author(s):  
Kevin B. Thurbide ◽  
C. M. Elson ◽  
P. G. Sim
Keyword(s):  
Carbon Dioxide ◽  
Mass Spectra ◽  
Chemical Ionization ◽  
Negative Ion ◽  
Ionization Mass ◽  
Structural Isomers ◽  
Mass Spectral ◽  
Negative Ion Chemical Ionization ◽  
Spectral Behaviour ◽  
Carbon Dioxide Plasma

The negative‒ion chemical ionization mass spectra of a group of structural isomers of amphetamine have been studied using carbon dioxide as the reagent gas. Characteristic and reproducible differences are observed for each member of the set implying that this technique offers a means of distinguishing among groups of amphetamine isomers. Characteristic adducts to the molecular ion are observed in the form (M–[H]+[O]) and (M–[H]+[CO2]). Descriptions of some fragments are given based on the mass spectral behaviour of a set of analogue compounds and the results of oxygen-18 labelled carbon dioxide reagent gas experiments. Contents of the carbon dioxide plasma and their impact on various analytes is also discussed.

scholarly journals Electron Impact Ionization Mass Spectra of 3-Amino 6-Chloro2-methyl Quinazolin-4-(3H)-one Derivative

2021 ◽  
pp. 1-5
Author(s):  
Osarumwense Peter Osarodion ◽  
◽  
Omotade Treasure Ejodamen ◽  
Keyword(s):  
Electron Impact ◽  
Mass Spectra ◽  
Impact Ionization ◽  
Cyclic Compound ◽  
Electron Impact Ionization ◽  
Ionization Mass ◽  
Fragmentation Pattern ◽  
Molecular Ion ◽  
Mass Spectral ◽  
Characteristic Fragmentation

Looking at the previous studies on quinazolinones derivatives, only limited information’s are available on their mass spectral along with the preparation of novel quinazolin-4-(3H)-one derivatives The condensation of Methyl-2-amino-4-Chlorobenzoate with acetic anhydride yielded the cyclic compound 2-methyl 7-Chloro-1, 3-benzo-oxazine-4-one (1) which further produce 3-Amino-2-Methyl 7-Chloro quinazolin-4(3H)-ones (2) via the reaction with hydrazine hydrate. The compounds synthesized were unequivocally confirmed by means of Infrared, Nuclear Magnetic Resonance (1H and 13C), Gas Chromatography-Mass spectrophotometry and Elemental analysis. Discussion: The molecular ion of m/z 235 fragments to give m/z 220 by loss of –NH group. The ion of m/z 220 was broken to give m/z 206 by losing CH2 group and fragment to m/z 177 by loss of HCO. This fragmented to m/z 162 by loss of –CH3 group and then m/z 136 by loss of CN group. The loss of O gave m/z 120 which fragment to give m/z 93 by loss of –HCN and finally gave m/z 65 by loss of CO group. Conclusion: The electron impact ionization mass spectra of compound 2show a weak molecular ion peak and a base peak of m/z 235resulting from a cleavage fragmentation. Compound 2 give a characteristic fragmentation pattern. From the study of the mass spectra of compound 2, it was found that the molecular ion had fragmented to the m/z 220. The final fragmentation led to ion of m/z 93 and ion of mass m/z 65, respectively

Electron ionization mass spectrometry of aryl- and fluoroalkyl-substituted palladium(II) β-diketonates and monothio-β-diketonates

1994 ◽  
Vol 72 (5) ◽  
pp. 1302-1311 ◽  
Author(s):  
Mark L. J. Reimer ◽  
John B. Westmore ◽  
Manoranjan Das
Keyword(s):  
Mass Spectra ◽  
Electron Ionization ◽  
Electron Ionization Mass Spectrometry ◽  
Ionization Mass ◽  
Aryl Group ◽  
Mass Spectral ◽  
Transition Series ◽  
Electron Ionization Mass Spectra ◽  
Positive Ion ◽  
Sulfur Donor

Positive ion electron ionization mass spectra are presented for palladium(II) β-diketonates and monothio-β-diketonates of the general form PdII[RC(X)CHC(O)R′]2, where R = phenyl, 4-methoxyphenyl, 2-thienyl, or 2-naphthyl; R′ = trifluoromethyl, pentafluoroethyl, or n-heptafluoropropyl; and X = O or S. The mass spectral behavior is in sharp contrast to that of metals of the first transition series. The spectra of the β-diketonates are dominated by metal-containing ions that arise by migration of the R group from the ligand (L) to palladium, but there is no evidence for fluorine-to-metal transfer. These findings are consistent with HSAB theory. The strong tendency of palladium to form bonds with unsaturated carbon also leads to remarkably abundant metal-containing ions that arise by losses of CO or aryloxy radicals from [PdRL]+• ions. In contrast, in decompositions of ions in the spectra of the monothio-β-diketonates, migration of the R group is suppressed; competition for palladium dπ electrons by the sulfur donor makes palladium a poorer aryl group acceptor.

scholarly journals Composition of the Essential Oil of Wild Growing Artemisia vulgaris from Erie, Pennsylvania

2012 ◽  
Vol 7 (5) ◽  
pp. 1934578X1200700 ◽  
Author(s):  
Jack D. Williams ◽  
Ayman M. Saleh ◽  
Dom N. Acharya
Keyword(s):  
United States ◽  
Essential Oil ◽  
The United States ◽  
Artemisia Vulgaris ◽  
Mass Spectral Analysis ◽  
Mass Spectral ◽  
Aerial Parts ◽  
Germacrene D ◽  
Leaf Oil ◽  
Chromatographic Mass

Essential Oil from wild growing Artemisia vulgaris L. originating in Erie, Pennsylvania was obtained by hydrodistillation of the aerial parts of the plant. Gas chromatographic-mass spectral analysis was used to identify the major volatiles present. Up to 22 components were detected in the essential oils. Germacrene D (25%), Caryophyllene (20%), α-Zingiberene (15%) and Borneol (11%) represent the major components of leaf oil, while the buds were rich in 1,8-Cineole (32%), Camphor (16%), Borneol (9%), and Caryophyllene (5%). trans-2-Hexenal was also detected in the aerial parts of the plant. α-Zingiberene and trans-2-Hexenal have not been previously reported for Artemisia vulgaris L. The major analytes are compared to those from Artemisia vulgaris L, originating outside of the United States.

scholarly journals Predicting in silico electron ionization mass spectra using quantum chemistry

2020 ◽  
Vol 12 (1) ◽  
Author(s):  
Shunyang Wang ◽  
Tobias Kind ◽  
Dean J. Tantillo ◽  
Oliver Fiehn
Keyword(s):  
Quantum Chemistry ◽  
In Silico ◽  
Mass Spectra ◽  
Large Scale ◽  
Computation Time ◽  
Molecular Size ◽  
Electron Ionization ◽  
Ionization Mass ◽  
Compound Identification ◽  
Mass Spectral

Abstract Compound identification by mass spectrometry needs reference mass spectra. While there are over 102 million compounds in PubChem, less than 300,000 curated electron ionization (EI) mass spectra are available from NIST or MoNA mass spectral databases. Here, we test quantum chemistry methods (QCEIMS) to generate in silico EI mass spectra (MS) by combining molecular dynamics (MD) with statistical methods. To test the accuracy of predictions, in silico mass spectra of 451 small molecules were generated and compared to experimental spectra from the NIST 17 mass spectral library. The compounds covered 43 chemical classes, ranging up to 358 Da. Organic oxygen compounds had a lower matching accuracy, while computation time exponentially increased with molecular size. The parameter space was probed to increase prediction accuracy including initial temperatures, the number of MD trajectories and impact excess energy (IEE). Conformational flexibility was not correlated to the accuracy of predictions. Overall, QCEIMS can predict 70 eV electron ionization spectra of chemicals from first principles. Improved methods to calculate potential energy surfaces (PES) are still needed before QCEIMS mass spectra of novel molecules can be generated at large scale.

Comparison of Gas Chromatographic/Mass Spectrometric and Liquid Chromatographic/Mass Spectrometric Methods for Confirmation of Coumaphos and Its Oxygen Analog in Eggs and Milk

1983 ◽  
Vol 66 (6) ◽  
pp. 1358-1364
Author(s):  
Kevin D White ◽  
Zhao Min ◽  
William C Brumley ◽  
Richard T Krause ◽  
James A Sphon
Keyword(s):  
Mass Spectra ◽  
Chemical Ionization ◽  
Negative Ions ◽  
Mass Spectrometric ◽  
Ionization Mass ◽  
Organophosphate Insecticide ◽  
Ion Detection ◽  
Oxygen Analog ◽  
Liquid Chromatographic ◽  
Chromatographic Mass

Abstract A comparison of a liquid chromatographic (LC)/mass spectrometric (MS) procedure for confirming coumaphos, an organophosphate insecticide, and its oxygen analog in milk and eggs with a capillary gas chromatographic (GO/MS method is presented. For the confirmation of coumaphos and its oxygen analog, multiple ion detection of both positive and negative ions from the chemical ionization mass spectra was used. Samples of milk and eggs fortified with the 2 compounds at the 0.1,0.01, and 0.005 ppm levels were analyzed. The major finding is the relatively greater efficiency of the LC/MS interface compared with the GC/MS capillary injector.

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