High resolution end group determination of low molecular weight polymers by matrix-assisted laser desorption ionization on an external ion source fourier transform ion cyclotron resonance mass spectrometer

Rooij, G.J. van; Duursma, Marc C.; Heeren, Ron M. A.; Boon, Jaap J.; Koster, Chris G. de

doi:10.1016/1044-0305(96)00003-7

Cited by 68 publications

(58 citation statements)

References 30 publications

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“…Their success is partly attributed to the extensive application of analytical tools such as liquid chromatography (LC), nuclear magnetic resonance spectroscopy and MS to characterize their structure. MS can provide structural information such as monomer unit and endgroup type [1][2][3][4], molecular weight distribution [5], monomer sequence and composition of copolymers [6][7][8]. This information is essential for polymer chemists, since knowledge of the microstructure of polymers enables the control of their synthesis and may provide the (cor)relation between structure and physicochemical and mechanical properties [9].…”

Section: Introductionmentioning

confidence: 99%

Electrospray ionization mass spectrometry of the non-covalent complexes of ammonium ions with high molar mass polyethers

Nasioudis

Velde

Heeren³

et al. 2011

International Journal of Mass Spectrometry

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Section: Introductionmentioning

confidence: 99%

Electrospray ionization mass spectrometry of the non-covalent complexes of ammonium ions with high molar mass polyethers

Nasioudis

Velde

Heeren³

et al. 2011

International Journal of Mass Spectrometry

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“…[8] The naming system used here is similar to that used in previous reports, [7a,f] that is, the series are named after their endgroup composition (Figure 2, [-H] indicating an unsaturated endgroup resulting from disproportionation.) The most intense series of peaks sh (or mh, which is one degree of polymerization (DP) higher than sh, but has the same elemental composition and therefore has the same mass as sh), m/z 439 + (nÀ3) 100, contains a butyl acetate endgroup (or methyl) at one end of the chain and is terminated with a H-abstracted endgroup at the other end.…”

mentioning

confidence: 98%

High‐Resolution Ion Mobility Spectrometry–Mass Spectrometry on Poly(methyl methacrylate)

et al. 2010

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Synthetic polymers are produced in industry to serve a global market across a wide range of areas.[1a-c] Increasingly complex polymeric structures have been developed to provide desirable properties and functions.[1d] The performance of these products depends on many factors such as endgroup composition, molecular weight distribution (MWD), and 3D conformation.[1e,f] Various analytical methods have been developed to obtain information about these properties. Conventional analytical techniques to study polymer systems include gel-permeation chromatography (GPC), [2a] Fourier-transform IR (FTIR), [2b] NMR spectroscopy, [2c] and differential scanning calorimetry (DSC).[2d]The development of "soft" ionization methods such as elecrospray ionization (ESI) [3a,b] and matrix-assisted laser desorption/ionization (MALDI) [3c,d] allowed mass spectrometry (MS) to become one of the most promising analytical methods for the analysis of polymeric systems. MS has the ability to characterize a dispersed polymer containing oligomers with different structures such as isomers or isobaric molecular weights. The combination of liquid chromatography (LC) and MS reduces the effects of ion suppression that may occur in an infusion MS analysis and provides an extra dimension of separation.[4] However, a relatively long separation time (> 30 min for HPLC, around 10 min for UPLC) is needed and a complex elution system using a variety of solvents has to be developed to suit a specific polymeric system.The combination of ion mobility spectrometry (IMS) and ESI-MS has been developed to analyze biomolecules and biopolymers.[5] Ion mobility describes how fast an ion in the gas phase moves through a drift cell that is filled with a carrier buffer gas under the influence of an electric field. More compact ions with a smaller collision cross-section will drift more quickly than expanded ions. The time-scale for separations in IMS is 100 ms to 10 ms, which is ideally suited for interfacing with an MS instrument. The extra dimension of separation based on drift time (t D ) provided by IMS is also highly complementary to the information obtained by MS. Although some studies on IMS-MS measurements of blends of disperse macromolecules, for example, poly(ethylene glycol) (PEG), have been reported, studies using IMS-MS on complex synthetic polymer systems are still limited. [6] Here, we demonstrate the power of using high resolution IMS-MS to study a poly(methyl methacrylate) (PMMA) synthesized by radical polymerization using peroxide initiator (tert-butyl peroxy-3,5,5-trimethylhexanoate) in solvent. Comprehensive studies on acrylic polymer produced by radical polymerization using MS have been done in the past decade. [7] It has been proven that high-resolution MS can discriminate between the effects of various polymerization mechanisms such as b-scission, chain transfer to solvent, radical transfer to solvent from the initiator, etc.[7] A system with complex endgroup combinations is expected since various initiation and termination reactions may ...

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“…51 Similarly, mixtures of alkali metal salts can produce well recognizable patterns ( Figure 5) and are useful in the analysis of polymers, especially those containing ether bonds. 52 Moreover, to facilitate cationization, special derivatives incorporating moieties with the high affinity to alkali ions (e.g. crown ethers) can also be employed.…”

Section: Cationizationmentioning

confidence: 99%

Fourier Transform-Ion Cyclotron Resonance-Mass Spectrometer as a New Tool for Organic Chemists

Pyrek¹

1999

Synlett

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Currently, mass spectral determination of molecular weights and elemental compositions of synthetic products is a common practice. It is aided by truly impressive developments in methods and instrumentation enabling to characterize great variety of compounds including even those of a relatively high molecular weight. Confidence in such measurements, however, depends upon selecting a suitable ionization method, unambiguous identification of a molecular-type ion, and the adequate precision of mass determinations. This review addresses major aspects of the ion formation and analysis with special attention given to the ion-cyclotron resonance. This powerful technique, different in its principle from most other methods of ion analysis, offers a superb combination of ion manipulation and measurement parameters and full compatibility with an array of ionization methods.Key words: mass spectrometry, ultra-high resolution mass spectrometry, ion-cyclotron-resonance, soft ionization, stable isotopes, molecular weight determination. Trapping ions in the ICR-cell 2.3.3.Detection of the trapped ions 2.3.4.Getting ions into the ICR Cell 2.4.Tandem mass spectrometry 2.4.1.Tandem mass spectrometry with magnetic-sectors and quadrupoles 2.4.2.Tandem-MS with FT-ICR-MS 3.Ion formation 3.1. Overview 3.2.Electron impact ionization 3.3.Chemical ionization 3.4.Fast atom bombardment 3.5.Matrix assisted laser desorption/ionization 3.6. Cationization 3.7.Electrospray ionization 4.Mass spectrometry and molecular weight determination 4.1.Stable isotopes and molecular ions 4.2.Isotopic depletion and substitution 4.3.High or ultra-high resolution? 4.4.Mass measurement accuracy 4.5.Can molecular weight be unequivocally determined by mass spectrometry? IntroductionMass spectrometry (MS) is the technique that renders mass-to-charge ratios (m/z) and relative intensities of ions formed (with exceptions), separated, and detected in the high vacuum. The remarkable analytical potentials of MS have been immediately recognized by its inventor J. J. Thomson and, in years immediately following the First World War, the detection and precise characterization of isotopes of almost all elements have been achieved employing the very first mass spectrographs and spectrometers. 1 With some delay, however, these seminal discoveries have been followed by a systematic effort to analyze organic compounds. Ever since, thanks to a steady progress in techniques and instrumentation, MS continues to serve in a variety of inorganic and organic applications. Moreover, by gaining truly astonishing capabilities in terms of ionization, mass range, sensitivity, and accuracy, MS methods cover classes of compounds that originally have been considered as entirely unsuitable for such an analysis.2 Still, as exemplified by the recent synthesis of two diterpenoids, 3 synthetic work can be carried out with the complete omission of MS. As a rule, however, MS data are used to confirm MW and to replace elemental analyses of the final reaction products. Only seldom, synthetic p...

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High resolution end group determination of low molecular weight polymers by matrix-assisted laser desorption ionization on an external ion source fourier transform ion cyclotron resonance mass spectrometer

Cited by 68 publications

References 30 publications

Electrospray ionization mass spectrometry of the non-covalent complexes of ammonium ions with high molar mass polyethers

Electrospray ionization mass spectrometry of the non-covalent complexes of ammonium ions with high molar mass polyethers

High‐Resolution Ion Mobility Spectrometry–Mass Spectrometry on Poly(methyl methacrylate)

Fourier Transform-Ion Cyclotron Resonance-Mass Spectrometer as a New Tool for Organic Chemists

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