The Mass Spectra of Imidoyl Halides and Bromoiminium Bromides

1973 ◽  
Vol 51 (1) ◽  
pp. 132-138 ◽  
Author(s):  
J. Gal ◽  
B. A. Phillips ◽  
R. Smith
Keyword(s):  
Mass Spectrometer ◽  
Alkyl Group ◽  
Mass Spectra ◽  
Halogen Atom ◽  
Fragmentation Pattern ◽  
Inlet System ◽  
Molecular Ion ◽  
Major Process ◽  
Hydrogen Rearrangement

The mass spectra of imidoyl halides 1–6 and bromoiminium bromides 7–9 have been studied and their fragmentation pattern discussed. Loss of halogen atom from the molecular ion of imidoyl halides to form a N-alkylnitrilium ion is a major process. When the N-alkyl group is larger than methyl the fragmentation of N-alkylnitrilium ions with hydrogen rearrangement to give the [PhC≡NH]+ ion becomes important. Thermolysis of bromoiminium bromides in the inlet system of the mass spectrometer produces imidoyl bromides via dealkylation (or dehydrobromination) and α,α-dibromobenzylamines via addition of bromide to the C=N bond.

scholarly journals Mass spectrometry analysis of polychlorinated biphenyls: Chemical ionization and selected ion chemical ionization using methane as a reagent gas

2000 ◽  
Vol 65 (5-6) ◽  
pp. 431-438 ◽  
Author(s):  
Tatjana Vasiljevic ◽  
Mila Lausevic ◽  
Raymond March
Keyword(s):  
Quantitative Analysis ◽  
Polychlorinated Biphenyls ◽  
Mass Spectrometer ◽  
Chemical Ionization ◽  
Quadrupole Ion Trap ◽  
Mass Spectrometry Analysis ◽  
Fragmentation Pattern ◽  
Gas Chromatograph ◽  
Molecular Ion ◽  
Fragment Ions

In the present paper a quadrupole ion trap mass spectrometer, coupled with a gas chromatograph, was used to compare the electron impact ionization (EI) and chemical ionization (Cl) technique, in terms of their selectivity in polychlorinated biphenyls (PCBs) quantitative analysis. The experiments were carried out with a modified Varian SATURN III quadrupole ion-storage mass spectrometer equipped with Varian waveform generator, coupled with a gas chromatograph with DB-5 capillary column. The disadvantage of using EI in the analysis of PCBs congeners is the extensive fragmentation of the molecular ion. The main fragmentation pattern recorded in the EI mass spectra of PCBs was the loss of a chlorine atom from the molecular ion. Therefore the fragment-ion signal overlapped with the molecular-ion cluster of lower mass congener. The fragmentation reactions of PCBs are suppressed if methane is used as a reagent gas for chemical ionization, but fragment ions are also present in the spectrum as an obstruction for quantitative analysis. The most selective method for PCBs quantitative analysis appears to be Cl with mass-selected C2H5 + ions from methane, which results in a mass spectrum with a negligible amount of fragment ions.

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

Mass Spectrometry of N-Benzoyl-2-hydroxyalkylamines. Role of the Hydroxylic Hydrogen in the Fragmentation Pattern

1975 ◽  
Vol 53 (21) ◽  
pp. 3175-3187 ◽  
Author(s):  
Don C. DeJongh ◽  
Denis C. K. Lin ◽  
Pierre LeClair-Lanteigne ◽  
Denis Gravel
Keyword(s):  
Mass Spectrometry ◽  
Mass Spectra ◽  
Hydroxyl Group ◽  
Fragmentation Pattern ◽  
Relative Importance ◽  
Hydrogen Atoms ◽  
Related Compounds ◽  
Double Hydrogen ◽  
Hydrogen Rearrangement

An interesting rearrangement has been observed in the mass spectra of a series of N-benzoyl-2-hydroxyalkylamines. The hydrogen atom of the hydroxyl group is transferred to the N-benzoyl portion of the molecular ion and the bond between positions 1 and 2 in the N-alkyl group is cleaved. A rearrangement ion, observed at m/e 135, is formed along with a neutral aldehyde or ketone. When the hydroxylic hydrogen is replaced by a trimethylsilyl substituent, the latter group is transferred with comparable efficiency. Differences in the relative importance of this rearrangement in the mass spectra of a series of related compounds with decreasing substitution at position 2, have been explained by differences in the stabilities of the neutral molecules formed along with m/e 135 and by the occurrence of a double hydrogen rearrangement which competes if hydrogen atoms are present in a relationship gamma and delta to the carbonyl group.

Thio derivatives of β-Diketones and their metal chelates. XV. Mass spectra of cobalt(III) and rhodium(III) chelates of some fluorinated Monothio-β-diketones

1974 ◽  
Vol 27 (6) ◽  
pp. 1177 ◽  
Author(s):  
M Das ◽  
SE Livingstone
Keyword(s):  
Thermal Degradation ◽  
Mass Spectrometer ◽  
Mass Spectra ◽  
Cobalt Complexes ◽  
Metal Chelates ◽  
Complex Ions ◽  
Molecular Ion ◽  
Derivatives Of ◽  
Bivalent State ◽  
Cobalt Chelates

The mass spectra of the cobalt(111) and rhodium(111) chelates of the fluorinated monothio-β-diketones RC(SH)=CHCOCF3 (R = Ph, p-MeC6H4, p-BrC6H4, p-FC6H4, and 2-thienyl) and of the cobalt(111) chelate of CH3C(SH)=CHCOCF3 have been obtained. The cobalt chelates do not give a peak for the molecular ion because of thermal degradation to the cobalt(11) complex CO(RCS=CHCOCF3)2, which then undergoes reactions in the mass spectrometer. Fluorine migration occurs with cobalt but not with rhodium. The cobalt complexes give rise to more metal-containing fragments than their rhodium analogues. Mechanisms are proposed for the reactions involving the metal-containing fragments. Cobalt undergoes valency changes to give cobalt(11) and cobalt(1) complex ions, whereas rhodium undergoes a valency change to the bivalent state only.

Thio derivatives of β-Diketones and their metal chelates. XVII. Mass spectra of iron(III) and ruthenium(III) chelates of some fluorinated Monothio-β-diketones

1974 ◽  
Vol 27 (10) ◽  
pp. 2115 ◽  
Author(s):  
M Das ◽  
SE Livingstone
Keyword(s):  
Thermal Degradation ◽  
Mass Spectrometer ◽  
Mass Spectra ◽  
Metal Chelates ◽  
Iron Chelates ◽  
Molecular Ion ◽  
Derivatives Of

The mass spectra of the iron(111) and rhodium(111) chelates of the fluorinated monothio-β-diketones RC(SH)=CHCOCF3 (R = Ph,p-MeC6H4, 2-thienyl) have been obtained. Whereas the ruthenium(111) chelates give a peak for the molecular ion, the iron(111) chelates do not, due to thermal degradation to the iron(11) complex Fe(RCS=CHCOCF3)2 which then undergoes reactions in the mass spectrometer. Fluorine migration occurs with two of the iron chelates but not with the ruthenium chelates. Mechanisms are proposed for the reactions of the ruthenium chelates.

Studies in Mass Spectrometry. II. Random Hydrogen Rearrangement in Aromatic Molecular Ions

1962 ◽  
Vol 15 (4) ◽  
pp. 771 ◽  
Author(s):  
CG Macdonald ◽  
JS Shannon
Keyword(s):  
Mass Spectrometry ◽  
Aromatic Compounds ◽  
Mass Spectra ◽  
Molecular Ions ◽  
Mass Spectrometric ◽  
Deuterium Exchange ◽  
Molecular Ion ◽  
Hydrogen Rearrangement ◽  
Aromatic Hydrogen

To provide data for investigations by, inter alia, mass-spectrometric methods into the deuterium exchange of the aromatic hydrogen of some coal fractions, a study was made which confirmed the occurrence of completely random hydrogen rearrangement prior to or during the elimination of C2H2 in the molecular ions of benzene-1,2,3-d3, benzene-l,3,5-d3, naphthalene-1,2,3,4-d4, naphthalene-1,4,5,8-d4, and phenanthrene-9,10-d2, and in the phenyl ions derived from o-bromobenzene-d, m-bromobenzene-d, and p-chlorobenzene-d, Similar but incomplete hydrogen rearrangement was found to occur in the molecular ion of carbazole-N-d prior to or during elimination of HCN. Such rearrangements, for which mechanistic considerations are presented, must be taken into account when the mass spectra of deuterium-substituted aromatic compounds are being interpreted.

scholarly journals Quadrupole Ion Trap Mass Spectrometer for Ice Giant Atmospheres Exploration

2021 ◽  
Vol 217 (1) ◽  
Author(s):  
J. Simcic ◽  
D. Nikolić ◽  
A. Belousov ◽  
D. Atkinson ◽  
C. Lee ◽  
...  
Keyword(s):  
Mass Spectrometer ◽  
Ion Trap ◽  
Quadrupole Ion Trap ◽  
Atomic Mass ◽  
Charge Ratio ◽  
Inlet System ◽  
Mass Spectrometers ◽  
Ion Trap Mass Spectrometer ◽  
Entry Probe ◽  
Composition Measurements

AbstractTo date, a variety of different types of mass spectrometers have been utilized on missions to study the composition of atmospheres of solar system bodies, including Venus, Mars, Jupiter, Titan, the moon, and several comets. With the increasing interest in future small probe missions, mass spectrometers need to become even more versatile, lightweight, compact, and sensitive.For in situ exploration of ice giant atmospheres, the highest priority composition measurements are helium and the other noble gases, noble gas isotopes, including 3He/4He, and other key isotopes like D/H. Other important but lower priority composition measurements include abundances of volatiles C, N, S, and P; isotopes 13C/12C, 15N/14N, 18O/17O/16O; and disequilibrium species PH3, CO, AsH3, GeH4, and SiH4. Required measurement accuracies are largely defined by the accuracies achieved by the Galileo (Jupiter) probe Neutral Mass Spectrometer and Helium Abundance Detectors, and current measurement accuracies of solar abundances.An inherent challenge of planetary entry probe mass spectrometers is the introduction of material to be sampled (gas, solid, or liquid) into the instrument interior, which operates at a vacuum level. Atmospheric entry probe mass spectrometers typically require a specially designed sample inlet system, which ideally provides highly choked, nearly constant mass-flow intake over a large range of ambient pressures. An ice giant descent probe would have to operate for 1-2 hours over a range of atmospheric pressures, possibly covering 2 or more orders of magnitude, from the tropopause near 100 mbar to at least 10 bars, in an atmospheric layer of depth beneath the tropopause of about 120 km at Neptune and about 150 km at Uranus.The Jet Propulsion Laboratory’s Quadrupole Ion Trap Mass Spectrometer (QITMS) is being developed to achieve all of these requirements. A compact, wireless instrument with a mass of only 7.5 kg, and a volume of 7 liters (7U), the JPL QITMS is currently the smallest flight mass spectrometer available for possible use on planetary descent probes as well as small bodies, including comet landers and surface sample return missions. The QITMS is capable of making measurements of all required constituents in the mass range of 1–600 atomic mass units (u) at a typical speed of 50 mass spectra per second, with a sensitivity of up to $10^{13}$ 10 13  counts/mbar/sec and mass resolution of $m/\Delta m=18000$ m / Δ m = 18000 at m/q = 40. (Throughout this paper we use the unit of m/q = u/e for the mass-to-charge ratio, where atomic mass unit and elementary charge are $1~\text{u} = 1.66\times 10^{-27}~\text{kg}$ 1 u = 1.66 × 10 − 27 kg and $1\text{e} = 1.6\times 10^{-19}$ 1 e = 1.6 × 10 − 19 C, respectively.) The QITMS features a novel MEMS-based inlet system driven by a piezoelectric actuator that continuously regulates gas flow at inlet pressures of up to 100 bar.In this paper, we present an overview of the QITMS capabilities, including instrument design and characteristics of the inlet system, as well as the most recent results from laboratory measurements in different modes of operation, especially suitable for ice giant atmospheres exploration.

Derivatization of polar organic compounds - performed directly in the inlet system of a mass spectrometer

1983 ◽  
Vol 48 ◽  
pp. 173-176 ◽  
Author(s):  
I. Fogy ◽  
H. Stipsits ◽  
E.R. Schmid ◽  
W. Kubelka
Keyword(s):  
Organic Compounds ◽  
Mass Spectrometer ◽  
Polar Organic Compounds ◽  
Inlet System

scholarly journals Mass Spectra of Oxygen-Nitrogen Plasma by Introduction of Organic Solvent in a Microwave Induced Plasma Mass Spectrometer.

1992 ◽  
Vol 8 (3) ◽  
pp. 375-376 ◽  
Author(s):  
Toshihiro SHIRASAKI ◽  
Kazuo YASUDA
Keyword(s):  
Organic Solvent ◽  
Mass Spectrometer ◽  
Mass Spectra ◽  
Nitrogen Plasma ◽  
Microwave Induced Plasma
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