Direct analysis in real time mass spectrometry of fused ring heterocyclic organometallic compounds

Mazzotta, Michael G.; Young, Jason O. E.; Evans, Jesse; Dopierala, Levi A.; Claytor, Z. A.; Smith, Adam C.; Snyder, Chad A.; Tice, Nathan C.; Smith, D.

doi:10.1039/c5ay00295h

Cited by 10 publications

(5 citation statements)

References 23 publications

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“…DART mass spectrometry also confirms the molecular mass of oxiranes 1 – 5 , with the expected [M+1]+ ion peak observed for each case. This observance is typical for positive scan mode in DART . Elemental analysis was performed for all previously unreported compounds (oxazines 2 , 4 , and 5 ).…”

Section: Resultsmentioning

confidence: 97%

“…The mass spectrometry analysis was performed with a direct analysis in real‐time SVP ion source (IonSense, Saugus, MA, USA) interfaced with a LTQ XL linear ion trap mass spectrometer (Thermo Scientific, San Jose, CA, USA). Specific details for this system and operation have been previously reported . All data reported here are under Positive Scan mode.…”

Section: General Experimentalmentioning

confidence: 99%

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Synthesis, Characterization, and Structure of Some 1,4‐Disubstituted Cyclopenta[d][1,2]oxazines

Tice

Collins

Smith

et al. 2017

Journal of Heterocyclic Chem

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Oxazine‐based chemistry offers an alternative to thiophene and pyrrole semiconductors and has been largely unexplored for electronics applications. Discrete monomers or oxazine polymers could serve as an efficient hole carrier for novel devices. A series of 1,4‐disubstituted cyclopenta[d][1,2]oxazines (R = tolyl, p‐nitrophenyl, t‐buytl, furyl, and 5‐methylthienyl) were isolated via ring closure with hydroxylamine from a 1,2‐acylcyclopentadiene precursor. The target oxazines were characterized by NMR and IR spectroscopy and direct analysis in real time (DART) MS. Single‐crystal x‐ray structure determination confirmed the identity of the tolyl oxazine, which shows a face‐to‐face stacking pattern of the heterocyclic rings.

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Section: Resultsmentioning

confidence: 97%

Section: General Experimentalmentioning

confidence: 99%

Synthesis, Characterization, and Structure of Some 1,4‐Disubstituted Cyclopenta[d][1,2]oxazines

Tice

Collins

Smith

et al. 2017

Journal of Heterocyclic Chem

Self Cite

View full text Add to dashboard Cite

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“…Mazzotta et al also reported the analysis of fused ring heterocyclic organometallic compounds using DART. 20…”

Section: Direct Analysis In Real Timementioning

confidence: 99%

Handling considerations for the mass spectrometry of reactive organometallic compounds

et al. 2022

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Mass spectrometry is a powerful tool in disparate areas of chemistry, but its characteristic strength of sensitivity can be an Achilles heel when studying highly reactive organometallic compounds. A quantity of material suitable for mass spectrometric analysis often represents a tiny grain or a very dilute solution, and both are highly susceptible to decomposition due to ambient oxygen or moisture. This complexity can be frustrating to chemists and analysts alike: the former being unable to get spec-

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“…DART emitter nozzles are typically positioned between 8 and 15 mm from the entrances of mass spectrometers. [50][51][52] The sample vial that delivers analyte vapour to the DART source was kept in the same position for all experiments (,1 cm below the capillary entrance to the mass spectrometer). The temperature of the capillary entrance to the mass spectrometer was set to 1508C, which is the minimum temperature that enabled the detection of benzylammonium in reasonably high abundances under these conditions.…”

Section: Dart Source Distance and Temperaturementioning

confidence: 99%

Internal Energy Deposition in Dielectric Barrier Discharge Ionization is Significantly Lower than in Direct Analysis in Real-Time Mass Spectrometry

2017

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The extent of internal energy deposition using three different plasma-based ionization mass spectrometry (MS) methods, atmospheric pressure chemical ionization (APCI), direct analysis in real time (DART), and active capillary dielectric barrier discharge ionization (DBDI), was investigated using benzylammonium 'thermometer' ions. Ions formed by DBDI were activated significantly less than those that were formed by DART and APCI under these conditions. Thermal ion activation by DART can be reduced slightly by positioning the DART source further from the capillary entrance to the MS and reducing the heat that is applied to metastable atoms exiting the DART source. For example, the average ion internal energy distribution decreased by less than 10 % (166.9 AE 0.3 to 152.2 AE 1.0 kJ mol À1) when the distance between the DART source and the MS was increased by 250 % (10 to 25 mm). By lowering the DART temperature from 350 to 1508C, the internal energy distributions of the thermometer ions decreased by ,15 % (169.93 AE 0.83 to 150.21 AE 0.52 kJ mol À1). Positioning the DART source nozzle more than 25 mm from the entrance to the MS and decreasing the DART temperature further resulted in a significant decrease in ion signal. Thus, varying the major DART ion source parameters had minimal impact on the 'softness' of the DART ion source under these conditions. Overall, these data indicate that DBDI can be a significantly 'softer' ion source than two of the most widely used plasma-based ion sources that are commercially available.

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Direct analysis in real time mass spectrometry of fused ring heterocyclic organometallic compounds

Abstract: Note demonstrates ability to gain analytical mass spectrometry data from organometallics without significant sample preparation or solubility issues for ionization.

Cited by 10 publications

References 23 publications

Synthesis, Characterization, and Structure of Some 1,4‐Disubstituted Cyclopenta[d][1,2]oxazines

Synthesis, Characterization, and Structure of Some 1,4‐Disubstituted Cyclopenta[d][1,2]oxazines

Handling considerations for the mass spectrometry of reactive organometallic compounds

Internal Energy Deposition in Dielectric Barrier Discharge Ionization is Significantly Lower than in Direct Analysis in Real-Time Mass Spectrometry

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