Analysis of air-,moisture- and solvent-sensitive chemical compounds by mass spectrometry using an inert atmospheric pressure solids analysis probe

Abstract

A novel method has been developed that enables chemical compounds to be transferred from an inert atmosphere glove box and into the atmospheric pressure ion source of a mass spectrometer whilst retaining a controlled chemical environment. This innovative method is simple and cheap to implement on some commercially available mass spectrometers. We have termed this approach inert atmospheric pressure solids analysis probe (iASAP) and demonstrate the benefit of this methodology for two air-/moisture-sensitive chemical compounds whose characterisation by mass spectrometry is now possible and easily achieved. The simplicity of the design means that moving between iASAP and standard ASAP is straightforward and quick, providing a highly flexible platform with rapid sample turnaround.

Keywords

Mass spectrometry inert atmospheric pressure solids analysis probe ionisation analysis moisture- and/or air-sensitive chemicals

Get full access to this article

View all access options for this article.

References

Deacon

Field

Fisher

et al.

Fullerene matrices in the MALDI-TOF mass spectroscopic characterization of organometallic compounds. J Organomet Chem 2014; 754: 482–492.

Linden

. Liquid injection field desorption ionization: A new tool for soft ionization of samples including air-sensitive catalysts and non-polar hydrocarbons. Eur J Mass Spectrom 2004; 10: 459–468.

Gross

Nieth

Linden

et al.

Liquid injection field desorption/ionization of reactive transition metal complexes. Anal Bioanal Chem 2006; 386: 52–58.

Lubben

McIndoe

Weller

. Coupling and electrospray ionization mass spectrometer with a glovebox: A straightforward, powerful and convenient combination for analysis of air sensitive organometallics. Organometallics 2008; 27: 3303–3306.

Ray

Bristow

Whitmore

et al.

On-line reaction monitoring by mass spectrometry, modern approaches for the analysis of chemical reactions. Mass Spec Rev. Epub ahead of print 19 May 2017. DOI: 10.1002/mas.21539.

Yan

Sokol

et al.

On-line reaction monitoring and mechanistic studies by mass spectrometry: Negishi cross-coupling, hydrogenolysis and reductive amination. Angew Chem Int Ed 2014; 53: 5931–5935.

Vikse

Woods

McIndoe

. Pressurized sample infusion for the continuous analysis of air and moisture-sensitive reactions using electrospray ionization mass spectrometry. Organometallics 2010; 29: 6615–6618.

McIndoe

. Mass spectrometry in organometallic chemistry. Spectrosc Prop Inorg Organomet Compd 2010; 41: 288–309.

McEwan

Ittel

. Field desorption mass spectrometry of air sensitive transition metal complexes. Org Mass Spectrom 1980; 15: 35–37.

10.

Eelman

Blacquiere

Moriarty

et al.

Shining new light on an old problem: Retooling MALDI mass spectrometry for organotransition-metal catalysis. Angew Chem Int Ed 2008; 47: 303–306.

11.

May

Marshall

. Inert gas purgebox for Fourier transform ion cyclotron resonance mass spectrometry of air-sensitive solids. Rev Sci Instrum 1994; 65: 612–616.

12.

Hoffmann

Schmidt

Scharsach

et al.

TG-MS of air-sensitive compounds in argon. Thermochim Acta 2012; 527: 204–210.

13.

Mosely JA, Dyer PW, Stokes P, et al. The analysis of air and solvent sensitive compounds using an Inert Atmospheric pressure Solids Analysis Probe (iASAP). In: The 31^st British Mass Spectrometry Society annual meeting, Cardiff, UK, 2010.

14.

Henderson

McIndoe

. Mass spectrometry of inorganic and organometallic compounds, Hoboken, NJ: Wiley, 2005.

15.

McEwan

McKay

Larsen

. Analysis of solids, liquids, and biological tissues using solids probe introduction at atmospheric pressure on commercial LC/MS instruments. Anal Chem 2005; 77: 7826–7831.

16.

Weston

. Ambient ionization mass spectrometry: Current understanding of mechanistic theory; analytical performance and application areas. Analyst 2010; 135: 661–668.

17.

Peacock

Zhang

Trimpin

. Advances in ionization for mass spectrometry. Anal Chem 2017; 89: 372–388.

18.

Horning

Carroll

et al.

New picogram detection system based on a mass spectrometer with an external ionization source at atmospheric pressure. Anal Chem 1973; 45: 936–943.

19.

Sunner

Nicol

Kebarle

. Factors determining relative sensitivity of analytes in positive mode atmospheric pressure ionization mass spectrometry. Anal Chem 1988; 60: 1300–1307.

20.

Smith

MJP

Cameron

Mosely

. Evaluating atmospheric pressure solids analysis probe (ASAP) mass spectrometry for the analysis of low molecular weight synthetic polymers. Analyst 2012; 137: 4524–4530.

21.

Stokes

Parker

Mosely

. Modification of a gas chromatography/atmospheric pressure chemical ionisation time-of-flight mass spectrometer as an alternative to automated atmospheric pressure solids analysis probe. Rapid Commun Mass Spectrom 2014; 28: 2024–2030.

22.

King

Sadanani

. Dialkylaminodichlorophosphines. Synth React Org Met Org Chem 1985; 15: 149–153.

23.

Schrock

Depue

Feldman

et al.

Further studies of imido alkylidene complexes of tungsten, well characterized olefin metathesis catalysts with controllable activity. Organometallics 1990; 9: 2262–2275.

24.

Cowley

Kemp

. Synthesis and reaction chemistry of stable two-coordinate phosphorus cations (phosphenium ions). Chem Rev 1985; 85: 367–382.

25.

Fang L, Dong C, Guo C, et al. Two competing ionisation processes in ESI-MS analysis of N-(1,3-diphenylallyl)benzenamines: Formation of the unusual [M-H]⁺ and the regular [M+H]⁺. Eur J Mass Spectrom. DOI: 10.1177/14690667177717228.

26.

Advion Inc. https://advion.com/products/expression/iasap-inert-analysis-probe/ (2017, accessed 12 July 2017).

Supplementary Material

Please find the following supplemental material available below.

For Open Access articles published under a Creative Commons License, all supplemental material carries the same license as the article it is associated with.

For non-Open Access articles published, all supplemental material carries a non-exclusive license, and permission requests for re-use of supplemental material or any part of supplemental material shall be sent directly to the copyright owner as specified in the copyright notice associated with the article.

0.00 MB

0.02 MB