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Porous and structured materials for dynamic nuclear polarization, process for their preparation and NMR analysis method

A structured, analyte-based technique, applied in control/regulation systems, measurements using electron paramagnetic resonance, instruments, etc., can solve problems such as no proof

Inactive Publication Date: 2015-04-15
UNIV CLAUDE BERNARD LYON 1 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has not proven to be a general method for detecting low concentrations of substrates in solution

Method used

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  • Porous and structured materials for dynamic nuclear polarization, process for their preparation and NMR analysis method
  • Porous and structured materials for dynamic nuclear polarization, process for their preparation and NMR analysis method
  • Porous and structured materials for dynamic nuclear polarization, process for their preparation and NMR analysis method

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Experimental program
Comparison scheme
Effect test

Embodiment approach

[0144] According to a preferred embodiment, the method comprises the following steps:

[0145] x) preparing the sample by mixing the analyte solution with the material of the invention,

[0146] xx) polarizing the sample by microwave irradiation, the free radicals attach to the material allowing the polarization,

[0147] xxx) Record the NMR spectrum of the polarized analyte.

[0148] Advantageously, the entire sample is cured before poling, and the poling of step xx) is performed on the cured sample. In a preferred embodiment, step xxx) is also carried out on the cured sample.

[0149] Steps xx) and xxx) are preferably performed in an NMR spectrometer, especially when step xx) and / or step xxx) is performed on a cured sample. This embodiment is easier to implement, but, at the time, it was possible to perform the polarization outside the spectrometer.

[0150] This method can also be performed by solution NMR. For example, a solidified sample can be polarized, but the NMR...

Embodiment 1

[0176] Example 1 - Mat-PrNHCO TEMPO with different dilutions - The dilutions given below correspond to the theoretical ratio defined as the amount of organic fragments in moles to the total amount of Si.

[0177] Preparation of Mat-PrN with different dilutions 3

[0178] Preparation of Mat-PrN 3 1 / 11

[0179] representative program

[0180] P123 (9.19 g) dissolved in aqueous HCl (365 mL, pH=1.5) was added to tetraethoxysilane (TEOS, 20.5 mL, 91.7 mmol) and 3-azidopropyltrimethyl Oxysilane (1.9 g, 9.3 mmol). The reaction mixture was stirred for 3 hours to obtain a microemulsion (clear mixture). To the reaction mixture heated at 45° C. was added a small amount of NaF (127 mg, 3 mmol) with stirring (composition of the mixture: 12 TEOS:1 of 3-azidopropyltriethoxysilane). The mixture was left under stirring at 45°C for 72 hours. The resulting solid was filtered and washed three times with 100 mL of water and three times with 100 mL of acetone. The surfactant was removed...

Embodiment 2

[0233] Example 2 - Mat-PrNHCO-Cyclohexyl TEMPO 1 / 35, which corresponds to the theoretical ratio defined as the amount of organic fragments in moles to the total amount of Si

[0234]

[0235] representative program

[0236] HBTU (79 mg, 0.21 mmol); HOBt (30 mg, 0.20 mmol); DIEA (0.11 mL, 0.64 mmol); 4-carboxy-cyclohexyl TEMPO (58 mg, 0.21 mmol) were used according to the above procedure; THF / DMF(50 / 50) (12ml / 12ml); Mat-PrNH 2 1 / 35 (401 mg); THF (40 mL) Prepare Mat-PrNHCO-cyclohexyl TEMPO 1 / 35; Mat-PrNHCO-cyclohexyl TEMPO 1 / 35 (352 mg). by N 2 Adsorption measurements yielded surface area = 640m 2 .g -1 ; Pore volume = 1.10 cm 3 .g -1 ; Average pore diameter = 9.2 nm. The hexagonal arrangement is known from XR-D.

[0237]

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Abstract

The present invention concerns materials consisting in a porous and structured network, this network being at least in part formed by Si atoms, or Si atoms and metal atoms, linked to each other's via siloxy bonds, the amount of radical ranging from 0.50 to 0.03 mmol of radical per gram of material, and in that the network is formed with a sol-gel step using an organosilane for the introduction of the organic molecules allowing their regular distribution within the porous structured material. The invention also concern a process for the preparation of such material and a method of analysis by Nuclear Magnetic Resonance (NMR) of an analyte wherein it uses dynamic nuclear polarization generated with a material according to the invention.

Description

technical field [0001] The present invention relates to the field of nuclear magnetic resonance (NMR) spectroscopy, and in particular to materials suitable for dynamic nuclear polarization (DNP). The present invention relates to new materials incorporating persistent free radicals covalently attached to structured and porous silica networks and methods of liquid state or nuclear magnetic resonance using such materials. Background technique [0002] Nuclear Magnetic Resonance (NMR) spectroscopy is a chemical analysis method that can reveal information about molecular structure and geometrical arrangement in space. However, NMR is an inherently insensitive analytical technique because the detected signal is proportional to the very weak particle population difference between the two nuclear levels. One way to improve the sensitivity is to increase the energy level difference by using a high magnetic field, the sensitivity increases with the magnetic field up to 3 / 2 the power....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01R33/28C08L83/04
CPCC08L83/08C08G77/26G01R33/282G01R33/4828G01R33/60
Inventor D·盖詹C·科佩雷特C·蒂欧勒克斯L·埃姆斯利A·勒萨热
Owner UNIV CLAUDE BERNARD LYON 1
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