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A temperature-jump design for conventional NMR probes
KTH, School of Chemical Science and Engineering (CHE), Chemistry, Physical Chemistry. KTH, School of Chemical Science and Engineering (CHE), Centres, Industrial NMR Centre.
KTH, School of Chemical Science and Engineering (CHE), Chemistry, Physical Chemistry. KTH, School of Chemical Science and Engineering (CHE), Centres, Industrial NMR Centre.ORCID iD: 0000-0002-0231-3970
2006 (English)In: Journal of magnetic resonance, ISSN 1090-7807, E-ISSN 1096-0856, Vol. 181, no 1, 148-153 p.Article in journal (Refereed) Published
Abstract [en]

 The design and performance of a simple probe insert for temperature-jump experiments in conventional NMR probes is described. The insert uses the output from conventional NMR amplifiers for heating conductive aqueous samples with a rate of 30-80 K/s for 200 W radiofrequency power. The observed dependence of the heating rate on sample conductivity is explained by the dominance of dielectric heating. Factors governing the temperature gradient within the sample are discussed.

Place, publisher, year, edition, pages
2006. Vol. 181, no 1, 148-153 p.
Keyword [en]
radiofrequency heating; radiofrequency coil; inductive heating; aqueous solution; liquid crystal; thermoresponsive polymer; phase transition; ethylene glycol; 59Co; cesium perfluorooctanoate
National Category
Chemical Sciences
Identifiers
URN: urn:nbn:se:kth:diva-5532DOI: 10.1016/j.jmr.2006.04.006ISI: 000238548000016OAI: oai:DiVA.org:kth-5532DiVA: diva2:9928
Note
QC 20100825Available from: 2006-04-05 Created: 2006-04-05 Last updated: 2017-11-21Bibliographically approved
In thesis
1. NMR Studies of Colloidal Systems in and out of Equilibrium
Open this publication in new window or tab >>NMR Studies of Colloidal Systems in and out of Equilibrium
2006 (English)Doctoral thesis, comprehensive summary (Other scientific)
Abstract [en]

The Thesis describes (i) the development of add-on instrumentation extending the capabilities of conventional NMR spectrometers and (ii) the application of the designed equipments and techniques for investigating various colloidal systems. The new equipments are:

Novel designs of stopped-flow and temperature–jump inserts intended for conventional Bruker wide-bore superconductive magnets. Both inserts are loaded directly from above into the probe space and can be used together with any 10 mm NMR probe with no need for any auxiliary instruments.

A set of 5 mm and 10 mm 1H – 19F – 2H NMR probes designed for heteronuclear 1H – 19F cross-relaxation experiments in Bruker DMX 200, AMX 300 and DMX 500 spectrometers, respectively.

A two–stage low-pass filter intended for suppressing RF noise in electrophoretic NMR experiments.

The kinetics of micellar dissolution and transformation in aqueous solutions of sodium perfluorooctanoate (NaPFO) is investigated using the stopped-flow NMR instrument. The sensitivity of NMR as detection tool for kinetic processes in micellar solutions is clarified and possible artefacts are analysed. In the NaPFO system, the micellar dissolution is found to proceed faster than 100 ms while surfactant precipitation occurs on the time scale of seconds-to-minutes. The kinetics of the coil-to–globule transition and intermolecular aggregation in a poly (Nisopropylacrylamide) solution are investigated by the temperature-jump NMR instrument. As revealed by the time evolution of the 1H spectrum, the T2 relaxation time and the self-diffusion coefficient D, large (>10 nm) and compact aggregates form in less than 1 second upon fast temperature increase and dissolve in less than 3 seconds upon fast temperature decrease.

The intermolecular 1H – 19F dipole-dipole cross-relaxation between the solvent and solute molecules, whose fast rotational diffusion is in the extreme narrowing limit, is investigated. The solutes are perfluorooctanoate ions either in monomeric or in micellar form and trifluoroacetic acid and the solvent is water. The obtained cross-relaxation rates are frequency-dependent which clearly proves that there is no extreme narrowing regime for intermolecular dipole-dipole relaxation. The data provide strong constraints for the dynamic retardation of solvent by the solute.

Place, publisher, year, edition, pages
Stockholm: KTH, 2006. 55 p.
Series
Trita-FYK, 0601
Keyword
stopped-flow NMR, temperature-jump NMR, crossrelaxation, NMR, NMR probe, fluorosurfactant, micellar kinetics, micellar structure
National Category
Physical Chemistry
Identifiers
urn:nbn:se:kth:diva-3898 (URN)91-7178-310-5 (ISBN)
Public defence
2006-04-20, Sal F3, Lindstedtsvägen 26, 10:00
Opponent
Supervisors
Note
QC 20100929Available from: 2006-04-05 Created: 2006-04-05 Last updated: 2010-09-29Bibliographically approved

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