NMR Measurement Method Preserving Magnetization for Time Resolution

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Solution Overview

Problem

Current time-resolved NMR measurement methods have low time resolution due to lengthy waiting times for magnetization recovery, making it difficult to observe fast chemical reactions or crystallization processes effectively.

Innovation Solution

The method involves performing one type of NMR measurement while preserving magnetization for the next, allowing subsequent measurements to start without waiting time, either immediately or concurrently, thereby reducing overall waiting time and increasing time resolution.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If conventional time-resolved NMR measurement is performed with full magnetization recovery waiting time between solution-state and solid-state measurements, then measurement reliability is ensured, but time resolution deteriorates significantly

Engineering Contradiction:
Improvemeasurement reliabilityVSAvoidtime resolution
Core Design Contradiction:
ReliabilityVSLoss of time

Solution Approach 1:

The patent applies preliminary action by performing solution-state NMR measurement first to preserve magnetization before conducting solid-state measurement. This sequence allows the second measurement to utilize remaining magnetization without requiring full recovery time, thereby reducing total measurement time while ensuring both measurements obtain sufficient signal quality

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent changes the measurement parameters by adjusting the number of scans and signal averaging strategies for each measurement type. Solution-state measurement uses fewer scans (e.g., 128) while solid-state uses more scans (e.g., 256), optimizing the balance between measurement speed and signal-to-noise ratio for each technique

Inventive Principle:
Principle #35Parameter changes

2Measurement precision

If the number of NMR signal acquisitions is increased to improve signal quality, then measurement precision improves, but measurement time increases

Engineering Contradiction:
Improvesignal qualityVSAvoidmeasurement time
Core Design Contradiction:
Measurement precisionVSLoss of time

Solution Approach 1:

The patent applies partial action by performing solution-state measurement with a smaller number of scans (128 times) compared to solid-state measurement (256 times). This partial approach is sufficient for solution-state due to stronger signals, while solid-state requires more scans for adequate signal quality, optimizing the balance between precision and time

Inventive Principle:
Principle #16Partial or excessive action

Solution Approach 2:

The patent maintains continuity of useful action by eliminating idle waiting time between solution-state and solid-state measurements. The solid-state measurement begins immediately after solution-state measurement completes, utilizing the preserved magnetization continuously without interruption, thereby reducing total measurement time while maintaining signal quality

Inventive Principle:
Principle #20Continuity of useful action

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This approach significantly reduces the total waiting time, potentially by half, enabling higher time resolution and the ability to observe fast processes that were previously unmeasurable.

Implementation Method 1

time-resolved nuclear magnetic resonance (NMR) measurement methods

Methodology Applied
Scientific EffectNuclear magnetic resonance: Magnetic Field

Implementation Method 2

The relaxation delay is 'waiting time' for recovering magnetization by forming a thermal equilibrium state in a static magnetic field

Methodology Applied
Scientific EffectMagnetization relaxation:

Implementation Method 3

cross polarization magic angle spinning (CP-MAS) measurement. More specifically, 1H is irradiated with a single pulse, and then, magnetization is transferred from 1H to 13C using CP

Methodology Applied
Scientific EffectCross polarization:

Implementation Method 4

magnetization is transferred from 1H to 13C using CP. Subsequently, an FID signal coming from 13C is observed. As dipole-dipole interaction is averaged due to molecular motion in the solution

Methodology Applied
Scientific EffectDipole-dipole interaction:

Implementation Method 5

The MAS method is a method for performing NMR measurement while spinning a container containing a sample, at high speed in a state in which the container is inclined at a predetermined angle (magic angle) with respect to the static magnetic field

Methodology Applied
Scientific EffectMagic angle spinning:

Data Source

PatentUS11067518B2NMR measurement method and apparatus
Publication Date: 2021.07.20 RIKEN CO LTD
  • US11067518B2 patent drawing
  • US11067518B2 patent drawing
  • US11067518B2 patent drawing

AI summary

A whole measurement process includes a plurality of step combinations. Each of the step combinations is composed of a solution-state measurement step and a solid-state measurement step. In the solution-state measurement step, solution-state NMR measurement is performed such that magnetization that is to be used in the solid-state measurement step remains. In the solid-state measurement step, solid-state NMR measurement is performed by using the magnetization that remains. No waiting time for recovering magnetization is provided between the solution-state measurement step and the solid-state measurement step. The solid-state measurement step may be performed earlier, and the solution-state measurement step may be performed later. Alternatively, the two steps may be performed simultaneously.