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      Going beyond electrospray: mass spectrometric studies of chemical reactions in and on liquids

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      Author(s): a , b , a ,
      Publication date (Electronic):
      Journal: Chemical Science
      Publisher: Royal Society of Chemistry

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          Abstract

          Recently developed and applied ionization techniques have brought mass spectrometry to bear on previously inaccessible chemistry. We offer our perspective on this field and its application for studying reaction mechanisms.

          Abstract

          There has been a burst in the number and variety of available ionization techniques to use mass spectrometry to monitor chemical reactions in and on liquids. Chemists have gained the capability to access chemistry at unprecedented timescales, and monitor reactions and detect intermediates under almost any set of conditions. Herein, recently developed ionization techniques that facilitate mechanistic studies of chemical processes are reviewed. This is followed by a discussion of our perspective on the judicious application of these and similar techniques in order to study reaction mechanisms.

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          Most cited references102

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          Fenton chemistry at aqueous interfaces.

          Shinichi Enami, Paul A Colussi, Yosuke Sakamoto (2014)
          In a fundamental process throughout nature, reduced iron unleashes the oxidative power of hydrogen peroxide into reactive intermediates. However, notwithstanding much work, the mechanism by which Fe(2+) catalyzes H2O2 oxidations and the identity of the participating intermediates remain controversial. Here we report the prompt formation of O=Fe(IV)Cl3(-) and chloride-bridged di-iron O=Fe(IV) · Cl · Fe(II)Cl4(-) and O=Fe(IV) · Cl · Fe(III)Cl5(-) ferryl species, in addition to Fe(III)Cl4(-), on the surface of aqueous FeCl2 microjets exposed to gaseous H2O2 or O3 beams for 10(3) times faster than Fe(H2O)6(2+) in bulk water via a process that favors inner-sphere two-electron O-atom over outer-sphere one-electron transfers. The higher reactivity of di-iron ferryls vs. O=Fe(IV)Cl3(-) as O-atom donors implicates the electronic coupling of mixed-valence iron centers in the weakening of the Fe(IV)-O bond in poly-iron ferryl species.
          Article 0 comments Cited 69 times – based on 0 reviews     Review now
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            Dynamic range of mass accuracy in LTQ Orbitrap hybrid mass spectrometer.

            Alexander Makarov, Eduard Denisov, Oliver Lange … (2006)
            Using a novel orbitrap mass spectrometer, the authors investigate the dynamic range over which accurate masses can be determined (extent of mass accuracy) for short duration experiments typical for LC/MS. A linear ion trap is used to selectively fill an intermediate ion storage device (C-trap) with ions of interest, following which the ensemble of ions is injected into an orbitrap mass analyzer and analyzed using image current detection and fast Fourier transformation. Using this technique, it is possible to generate ion populations with intraspectrum intensity ranges up to 10(4). All measurements (including ion accumulation and image current detection) were performed in less than 1 s at a resolving power of 30,000. It was shown that 5-ppm mass accuracy of the orbitrap mass analyzer is reached with >95% probability at a dynamic range of more than 5000, which is at least an order of magnitude higher than typical values for time-of-flight instruments. Due to the high resolving power of the orbitrap, accurate mass of an ion could be determined when the signal was reliably distinguished from noise (S/Np-p)>2...3).
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              Effect of different solution flow rates on analyte ion signals in nano-ESI MS, or: when does ESI turn into nano-ESI?

              Andrea Schmidt, Michael Karas, Thomas Dülcks (2003)
              In nano-ESI MS, the qualitative and quantitative characteristics of mass spectra vary considerably upon the use of different spraying conditions, i.e., aperture of the spraying needle and the voltage applied. The major parameters affected by the aperture size is the liquid flow rate which determines the initial droplet size and the current emitted upon the spray process, as described by different models of the ESI process. In the present study, the effect of flow rate on ion signals was studied systematically using mixtures of compounds with different physicochemical properties (i.e., detergent/oligosaccharide and oligosaccharide/peptide). For these model systems, the functional dependence of certain analyte-ion ratios upon the flow rate can be correlated to changes in analyte partition during droplet fission prior to ion release. Analyte suppression is practically absent at minimal flow rates below 20 nL/min.
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                Author and article information

                Journal
                Journal ID (nlm-ta): Chem Sci
                Journal ID (iso-abbrev): Chem Sci
                Title: Chemical Science
                Publisher: Royal Society of Chemistry
                ISSN (Print): 2041-6520
                ISSN (Electronic): 2041-6539
                Publication date (Print): 1 January 2016
                Publication date (Electronic): 1 October 2015
                Volume: 7
                Issue: 1
                Pages: 39-55
                Affiliations
                [a ] Department of Chemistry , Stanford University , Stanford , CA 94305 , USA . Email: zare@ 123456stanford.edu
                [b ] Thermo Fisher Scientific , San José , CA 95134 , USA
                Article
                Publisher ID: c5sc02740c
                DOI: 10.1039/c5sc02740c
                PMC ID: 5508663
                PubMed ID: 28757996
                SO-VID: caec5b39-ca20-4ede-a0bd-51853840ed1d
                Copyright © This journal is © The Royal Society of Chemistry 2015
                License:

                This is an Open Access article distributed under the terms of the Creative Commons Attribution 3.0 Unported License ( http://creativecommons.org/licenses/by/3.0/) which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

                History
                Date received : 27 July 2015
                Date accepted : 1 October 2015
                Categories
                Subject: Chemistry

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