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US4774467A
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Method for recording nuclear magnetic resonance spectra
Assignee: Spectrospin AG
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Filing: 1986-12-04
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Granted: 1988-09-27
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Expires: 2006-12-04
Abstract
Abstract To eliminate homonuclear couplings along the ω 1 axis in 2D spectroscopy, a time reversal pulse (5, 6) is inserted into the pulse sequence that is generally employed for experiments of this type, which time reversal pulse divides the evolution period t 1 that is required for experiments of this type into two equal portions. The time reversal pulse is intended to cause the spin moments to rotate about an angle β n and is preferably composed of two 90° pulses, the first of which has a phase of β n +φ q and the second a phase of π+φ q . The phase of the RF oscillation of the pulse that precedes the time reversal must be shifted by an angle of β n . A plurality of 3(2N-1) of these signals having different phases are added together after being weighted by a factor which preferably amounts to ##EQU1##
Inventors
- 👤 Ole W. Sorensen
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-07 10:59
CPC Classifications
G; G01; G01R; G01R33/00; G01R33/20; G01R33/44; G01R33/46; G01R33/4633
Claims Analysis
Total Claims: 8
Claim 1
Independent Claim
302 words
A method for recording the nuclear magnetic resonance spectra of molecular spin systems between which there is an interactive effect in which said spin systems are excited by means of a 90° pulse and the resonance signals of the excited spin systems are not observed until the end of an evolution period t 1 that follows the 90° pulse, wherein said spin system is irradiated with a time reversal pulse after one half of the evolution period (t 1 /2), with said time reversal pulse causing the spin moments to rotate by a flip angle β n and their RF oscillation to have a phase shift of φ q relative to a reference phase, while the RF oscillation of all pulses that precede said time reversal pulse have a phase shift of ψ+β n relative to said reference phase, in which phase shift ψ represents either 0 or π and β n coincides with said flip angle of said time reversal pulse and is determined by the maximum number N of coupled spins in said spin system, in accordance with the equation ##EQU13## wherein n=0, 1, 2, . . . , N-1, N+1, . . . , 2N-1 while φ q independently of β n assumes one of the values ##EQU14## wherein q=0, 1, 2, and in that signals which are received on the basis of 3(2N-1) excitations, are multiplied by a weighting factor of ##EQU15## and then added together to form a resulting signal, which weighting factor is the Fourier transformation of the factors ##EQU16## in which K represents the highest number of couplings that are actually present in said spin system and p represents a continuously changing integer between 0 and K, so that ##EQU17## while δ K ,N has a value of 1 if N=K, and otherwise is zero.
Claim 2
Independent Claim
302 words
A method for recording the nuclear magnetic resonance spectra of molecular spin systems between which there is an interactive effect in which said spin systems are excited by means of a 90° pulse and the resonance signals of the excited spin systems are not observed until the end of an evolution period t 1 that follows the 90° pulse, wherein said spin system is irradiated with a time reversal pulse after one half of the evolution period (t 1 /2), with said time reversal pulse causing the spin moments to rotate by a flip angle β n and their RF oscillation to have a phase shift of φ q relative to a reference phase, while the RF oscillation of all pulses that precede said time reversal pulse have a phase shift of ψ+β n relative to said reference phase, in which phase shift ψ represents either 0 or π and β n coincides with said flip angle of said time reversal pulse and is determined by the maximum number N of coupled spins in said spin system, in accordance with the equation ##EQU13## wherein n=0, 1, 2, . . . , N-1, N+1, . . . , 2N-1 while φ q independently of β n assumes one of the values ##EQU14## wherein q=0, 1, 2, and in that signals which are received on the basis of 3(2N-1) excitations, are multiplied by a weighting factor of ##EQU15## and then added together to form a resulting signal, which weighting factor is the Fourier transformation of the factors ##EQU16## in which K represents the highest number of couplings that are actually present in said spin system and p represents a continuously changing integer between 0 and K, so that ##EQU17## while δ K ,N has a value of 1 if N=K, and otherwise is zero.
Claim 3
Dependent Claim
53 words
The method according to claim 1, wherein said time reversal pulse has a first portion in the form of a 90° pulse having a phase of β n +φ q and a second portion which follows said first portion in the form of a 90° pulse having a phase of π+φ q .
Claim 4
Dependent Claim
56 words
The method according to claim 1 or 2, wherein pulse sequences are employed which are suitable for recording two-dimensional nuclear magnetic resonance spectra and have an inserted time reversal pulse, and in which the phase of the RF oscillation of the excitation pulse that precedes the time reversal pulse is shifted by angle β n .
Claim 5
Dependent Claim
51 words
The method according to claim 3, wherein the pulse sequence is 90°(β.sub.n +ψ.sub.1)-1/2t.sub.1 -90°(β.sub.n +φ.sub.q)-τ-90°(π+φ.sub.q)-1/2t.sub.1 -90°(0)-τ.sub.m -90°(ψ.sub.2)-acq. (ψ.sub.1 +ψ.sub.2), wherein ψ 1 and ψ 2 are alternatively 0 and π in a cycle that is independent of β and φ and τ m is the variable mixing time of NOESY experiments.
Claim 6
Dependent Claim
62 words
The method according to claim 3 for investigation of spin systems with heteronuclear coupling, in which a first kind of nuclei is directly excited by a first pulse sequence and then the excitation by coupling of a second kind of nuclei is examined by means of a second pulse sequence, wherein the time reversal pulse is inserted into said first pulse sequence.
Claim 7
Dependent Claim
199 words
The method according to claim 3 for indirect investigation of spin systems with heteronuclear coupling in which a first kind of nuclei is excited by means of a first pulse sequence and a second kind of nuclei is excited by means of a second pulse sequence in such a manner that a first 180° pulse following a first 90° pulse of said first pulse sequence is centered between two 90° pulses of said second pulse sequence, wherein said time reversal pulse is inserted in said first pulse sequence at a location that is in time coincidence with said second 90° pulse of said second pulse sequence, wherein said time reversal pulse is followed by a further 180° pulse after a time interval that is identical to the time interval between said first 90° pulse and said first 180° pulse, and wherein scanning of the resonance signal provided by said first kind of nuclei starts after a time interval from said further 180° pulse that is identical to the time interval between said first 180° pulse and said time reversal pulse, so that said time reversal pulse is centered between said first 90° pulse and start of said signal scanning.
Claim 8
Dependent Claim
38 words
The method according to claim 2 in which the second portion of the time reversal pulse follows the first portion of the time reversal pulse in a time interval τ which is short relative to the evolution period.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1991-09-27 | 1992-03-28 | 1992-09-27 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1995-09-27 | 1996-03-28 | 1996-09-27 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1999-09-27 | 2000-03-28 | 2000-09-27 | $7700.00 | Window Closed / Lapsed |