NMR Spectrometer Microchip Reactor Solvent Consumption

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Solution Overview

Problem

NMR spectrometers require large amounts of expensive deuterated solvent for locking and necessitate frequent adjustments in resolution when samples are exchanged, leading to high operating costs and inefficiencies.

Innovation Solution

An NMR spectrometer with a microchip reactor that allows for the introduction and reaction of reagents within a sample tube holding deuterated solvent, enabling reduced solvent usage and eliminating the need for resolution adjustments during sample exchanges by using a microchip reactor with channels for mixing and reacting reagents without mixing with the deuterated solvent.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Loss of substance

If a coaxial sample tube is used to separate sample and deuterated compound, then the expensive deuterated compound can be reused and measurement costs are suppressed, but the resolution of the instrument needs to be readjusted whenever sample exchange is made

Engineering Contradiction:

Improvedeuterated compound consumptionVSAvoidresolution adjustment frequency

Core Design Contradiction:

Loss of substanceVSEase of operation

Solution Approach 1:

The sample tube is divided into two separate compartments: an inner tube for containing the sample and an outer tube for containing the deuterated compound. This segmentation allows the deuterated compound to remain stationary and reusable while the sample can be exchanged without disturbing the deuterated compound, eliminating the need for resolution readjustment during sample exchange.

Inventive Principle:

Principle #1Segmentation

2Productivity

If an auto-sample changer is used to perform successive measurements, then labor is reduced, but sample tubes must be inserted and withdrawn during exchange which requires resolution readjustment and deuterated compound to be added to every sample tube

Engineering Contradiction:

Improvemeasurement efficiencyVSAvoiddeuterated compound consumption

Core Design Contradiction:

ProductivityVSLoss of substance

Solution Approach 1:

The outer tube containing the deuterated compound serves multiple functions: it provides NMR locking signal for the entire measurement session, acts as a reusable component that doesn't need to be replaced with each sample exchange, and maintains a stable magnetic environment. This multi-functionality eliminates the need to add deuterated compound to every sample tube and reduces overall consumption.

Inventive Principle:

Principle #6Universality (Multi-functionality)

3Ease of operation

If a flow NMR probe is used for continuous delivery of liquid, then sample tubes do not need to be inserted and withdrawn so resolution needs to be adjusted only once, but a large amount of deuterated solvent is necessary for NMR locking and cleaning and expensive dedicated probes are required

Engineering Contradiction:

Improveresolution adjustment frequencyVSAvoiddeuterated solvent consumption

Core Design Contradiction:

Ease of operationVSLoss of substance

Solution Approach 1:

The deuterated compound is extracted from the sample tube and placed in a separate outer tube. This allows the deuterated compound to be reused across multiple sample measurements without being consumed or contaminated by the sample, significantly reducing the amount needed compared to traditional methods where deuterated solvent is required for both locking and cleaning.

Inventive Principle:

Principle #2Taking out (Extraction)

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 minimizes deuterated solvent consumption and eliminates the need for frequent resolution adjustments, reducing operating costs and enhancing measurement efficiency by allowing continuous use of the deuterated solvent independent of the sample solvent.

Implementation Method 1

The introduction portion has an introduction channel for introducing a reagent introduced from the outside into the reaction portion and a discharge channel for permitting the reaction liquid discharged from the reaction portion to be discharged to the outside

Methodology Applied

Scientific EffectFluid flow through microchannels:

Implementation Method 2

detecting the amount of shift of the position of the NMR signal originated from the deuterium nucleus due to drift in the static magnetic field

Methodology Applied

Scientific EffectNMR signal detection:

Implementation Method 3

feeding back a signal corresponding to the shift to the shim coil current used to superimpose a correcting magnetic field on the static magnetic field

Methodology Applied

Scientific EffectMagnetic field drift correction:

Implementation Method 4

a magnet for producing a static magnetic field for NMR measurements

Methodology Applied

Scientific EffectStatic magnetic field generation: Magnetic Field

Data Source

PatentUS7463032B2NMR spectrometer and method of NMR measurement

Publication Date: 2008.12.09 JEOL LTD

AI summary

There is disclosed a microchip reactor-type apparatus for effecting organic synthesis and reactions. The apparatus can be used in combination with many analytical instruments. The apparatus has a magnet for producing a static magnetic field for NMR measurements, a sample tube placed within the static magnetic field and holding a deuterated solvent therein, and a microchip reactor inserted inside the sample tube. A sample solution to be investigated is introduced into the channel formed in the microchip reactor while the microchip reactor is inserted inside the sample tube holding the deuterated solvent therein.