Method and apparatus for increasing the detection sensitivity in a high resolution NMR analysis
First Claim
1. A method of increasing the detection sensitivity of a high resolution NMR analysis comprising the steps of:
- a) preparing a solution by dissolving an NMR sample material in a liquid solvent comprising molecular substance capable of forming a photo-excited triplet state molecules when exposed to optical radiation,b) applying a magnetic field to said solution;
c) freezing said solution for forming a frozen solution being a solid substance;
d) exposing said frozen solution to optical radiation for exciting the triplet state molecules therein;
e) exposing said frozen solution to microwave radiation for exciting spin transitions in said triplet state molecules and causing dynamic nuclear polarization of at least one nuclear species of the frozen solution;
f) melting said frozen solution by applying heat thereto; and
g) analyzing said NMR sample material by performing an NMR analysis of the at least one polarized nuclear species.
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Abstract
Enhanced nuclear polarization of a magnetic resonance sample provides greater detection sensitivity over conventional NMR spectroscopy due to a method and an apparatus of increasing the detection sensitivity. Molecules capable of forming photo-excited triplet states are combined in a solution with a NMR sample. While in a uniform magnetic field the solution is frozen, optical radiation is applied to produce photo-excited triplet states molecules and a microwave radiation is applied to stimulate transitions of one of the triplet lines producing dynamic polarization of the nuclei in the magnetic resonance sample. The frozen sample is then rapidly melted and a NMR analysis is performed.
49 Citations
18 Claims
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1. A method of increasing the detection sensitivity of a high resolution NMR analysis comprising the steps of:
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a) preparing a solution by dissolving an NMR sample material in a liquid solvent comprising molecular substance capable of forming a photo-excited triplet state molecules when exposed to optical radiation, b) applying a magnetic field to said solution; c) freezing said solution for forming a frozen solution being a solid substance; d) exposing said frozen solution to optical radiation for exciting the triplet state molecules therein; e) exposing said frozen solution to microwave radiation for exciting spin transitions in said triplet state molecules and causing dynamic nuclear polarization of at least one nuclear species of the frozen solution; f) melting said frozen solution by applying heat thereto; and g) analyzing said NMR sample material by performing an NMR analysis of the at least one polarized nuclear species. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12)
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13. A method of producing enhanced nuclear polarization of a NMR sample for performing an NMR analysis comprising the steps of:
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dissolving a NMR sample in a liquid solvent comprising photo-excitable triplet state molecules; freezing said liquid solvent for obtaining a solid substance; exposing said solid substance in a presence of a magnetic field to optical radiation forming photo-excited triplet state molecules; exposing said solid substance to microwave radiation polarizing one or more nuclei of the NMR sample by transferring energy thereto from the photo-excited triplet state molecules; and performing the NMR analysis of at least one polarized nuclear species of the NMR sample in a melted solvent. - View Dependent Claims (14)
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15. An NMR apparatus for performing a method of increasing detection sensitivity of high resolution NMR analysis comprising:
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a sample cell being transparent to RF, microwave, and optical radiation and comprising a liquid solvent having molecular substance capable of forming a photo-excited triplet state molecules upon exposure to optical radiation with NMR sample dissolving therein; a dewar surrounding said sample cell and being transparent to RF, microwave, and optical radiation; a cold and a warm fluid sources coupled to the dewar providing respectively cold and warm fluid to an exterior of the sample cell; an RF coil mounted on an outer surface of the dewar and providing RF field in a selected region of the sample cell; an optical source producing optical radiation onto the sample cell a magnet providing a magnetic field in the region of the sample cell a microwave spectrometer; a microwave structure coupled to the microwave spectrometer, which provides microwave magnetic field in the region of the sample; an NMR spectrometer connected to the RF coil, which detects NMR signals induced in the RF coil; and a computer programmed in assistance to perform the steps of freezing the solution to a solid substance;
exposing it to optical and microwave radiation for obtaining photo-excited triplet state molecules that transfers their energy to the NMR sample causing dynamic nuclear polarization of at least one nuclear species of the NMR sample, melting the frozen solution and analyzing the NMR sample. - View Dependent Claims (16, 17, 18)
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Specification