Temperature-programmed packed capillary liquid chromatography coupled to evaporative light-scattering detection and electrospray ionization time-of-flight mass spectrometry for characterization of high-molecular-mass hindered amine light stabilizers

Andersen, Thomas; Skuland, Inger Lill; Holm, Anders; Trones, Roger; Greibrokk, Tyge

doi:10.1016/j.chroma.2003.12.043

Cited by 41 publications

(28 citation statements)

References 39 publications

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“…The development of new ionization techniques promoted MS for highly sensitive and selective detection [10,[20][21][22]24]. Compared with MS, IR detection lost its importance [23].…”

Section: Chromatographic Procedures For Stabilizersmentioning

confidence: 99%

Analysis of polyolefin stabilizers and their degradation products

Reingruber

Buchberger

2010

J of Separation Science

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Polymeric materials are complex samples, as they contain various groups of additives, compounding ingredients, and fillers. An important group of additives are stabilizers. Efficient stabilization is essential especially for polypropylene, as it is sensitive to oxidation and radical attack due to the numerous tertiary carbon atoms in its structure. How long a polymer will be sufficiently stabilized can be deduced from the contained amount of intact stabilizer. Different approaches for the analysis of stabilizers in polyolefins are available, which include sample preparation with subsequent chromatographic separation as well as direct analysis techniques. In round-robin tests, stabilizer concentrations obtained varied strongly. This shows the demand for reliable and robust methods. Stabilizers get consumed while protecting the polymer and are then present as degradation products. They were observed while quantifying intact stabilizers, in migration studies, and - if volatile - in emission studies of polymers. Furthermore, e.g. interactions with other polymer ingredients or irradiation degraded stabilizers. The identification of degradation products provides a better insight into the reactions associated with stabilization. Their quantitation makes it possible to deduce the original level of stabilization. Furthermore, polymer ingredients degrading stabilizers can be identified. Knowledge on these interactions contributes significantly to improved polymer stabilization.

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“…The development of new ionization techniques promoted MS for highly sensitive and selective detection [10,[20][21][22]24]. Compared with MS, IR detection lost its importance [23].…”

Section: Chromatographic Procedures For Stabilizersmentioning

confidence: 99%

Analysis of polyolefin stabilizers and their degradation products

Reingruber

Buchberger

2010

J of Separation Science

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“…LC-MS can, however, suffer from relatively long analysis times that can be prohibitive in studies involving large numbers of samples. [16] Taguchi et al have described a novel solvent-less preparation technique for matrix-assisted laser desorption ionisation (MALDI) mass spectrometry which was used to directly analyse oligomeric HALS in polymers. [17 -19] Polypropylene samples impregnated with HALS were frozen with liquid nitrogen and then milled in the presence of the ionisation matrix.…”

Section: Introductionmentioning

confidence: 99%

Structural identification of hindered amine light stabilisers in coil coatings using electrospray ionisation tandem mass spectrometry

et al. 2010

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Hindered amine light stabilisers (HALS) are the most effective antioxidants currently available for polymer systems in post-production, in-service applications, yet the mechanism of their action is still not fully understood. Structural characterisation of HALS in polymer matrices, particularly the identification of structural modifications brought about by oxidative conditions, is critical to aid mechanistic understanding of the prophylactic effects of these molecules. In this work, electrospray ionisation tandem mass spectrometry (ESI-MS/MS) was applied to the analysis of a suite of commercially available 2,2,6,6-tetramethylpiperidine-based HALS. Fragmentation mechanisms for the [M + H](+) ions are proposed, which provide a rationale for the product ions observed in the MS/MS and MS(3) mass spectra of N-H, N-CH(3), N-C(O)CH(3) and N-OR containing HALS (where R is an alkyl substituent). A common product ion at m/z 123 was identified for the group of antioxidants containing N-H, N-CH(3) or N-C(O)CH(3) functionality, and this product ion was employed in precursor ion scans on a triple quadrupole mass spectrometer to identify the HALS species present in a crude extract from of a polyester-based coil coating. Using MS/MS, two degradation products were unambiguously identified. This technique provides a simple and selective approach to monitoring HALS structures within complex matrices.

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“…The drift could be corrected mathematically [104]. The compatibility between temperature programming in LC and MS was shown a decade ago [134], and recently also with electrospray ionization [107,117]. Since temperature programming can be expected to affect the ionization process in electrospray ionization less than solvent gradients, tem-perature programmed LC-MS may in many cases be a better choice than using solvent gradient LC-MS, where addition of sheath liquids may be necessary to maintain the sensitivity throughout the gradient.…”

Section: Instrumentationmentioning

confidence: 99%

Controlling the retention in capillary LC with solvents, temperature, and electric fields

Jandera

Blomberg

Lundanes³

2004

J of Separation Science

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Once a suitable stationary phase and column dimensions have been selected, the retention in liquid chromatography (LC) is traditionally adjusted by controlling the mobile phase composition. Solvent gradients enable achievement of good separation selectivity while decreasing the separation time as compared to isocratic elution. Capillary columns allow use of other programming parameters, i.e. temperature and applied electric fields, in addition to solvent gradient elution. This paper presents a review of programmed separation techniques in miniaturized LC, including retention modeling and method transfer from the conventional to micro- and capillary scales. The impact of miniaturized instrumentation on retention and the limitations of capillary LC are discussed. Special attention is focused on the gradient dwell volume effects, which are more important in micro-LC techniques than in conventional analytical LC and may cause significant increase in the time of analysis, unless special instrumentation and (or) pre-column flow-splitting is used. The influence of temperature upon retention is also discussed, and applications where the temperature has been actively used for retention control in capillary LC are included together with the instrumentation utilized. Finally the possibilities of additional selectivity control by applying an electric field over a packed capillary LC column are discussed.

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Temperature-programmed packed capillary liquid chromatography coupled to evaporative light-scattering detection and electrospray ionization time-of-flight mass spectrometry for characterization of high-molecular-mass hindered amine light stabilizers

Cited by 41 publications

References 39 publications

Analysis of polyolefin stabilizers and their degradation products

Analysis of polyolefin stabilizers and their degradation products

Structural identification of hindered amine light stabilisers in coil coatings using electrospray ionisation tandem mass spectrometry

Controlling the retention in capillary LC with solvents, temperature, and electric fields

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