RU1826072C - Cell for carrying out nmr-measurements in liquids and gases under pressure - Google Patents

Abstract

Application: field of technical physics, research and analysis of materials by NMR. The essence of the invention: a cell for NMR measurements consists of a segment of a quartz tube with a hole, a valve in the form of a disk of vacuum rubber with a diameter equal to the inner diameter of the ampoule is inserted inside the ampoule. The ability to adjust the pressure and concentration of the substance upon introduction of the valve allows expanding the functionality of NMR spectrometers and also simplifies the process of sample preparation. 1 ill.

Description

The invention relates to the field of technical physics and is related to the study and analysis of materials using NMR methods.

The purpose of the invention is the expansion of the functionality of serial NMR spectrometers not specifically designed for working with samples in which the pressure and concentration of the starting materials are required to be controlled, maintained or changed during the experiment, as well as simplification of the sample preparation process and an increase in the accuracy of pressure setting and concentrations of starting materials in the samples.

The ampoule device is shown in the drawing.

It is a piece of quartz tube 1 with a length of 50 mm with an outer diameter of 4 to 9 mm and a wall thickness of 1 mm. One end of the tube is sealed tightly; at the other, hole 2 with a diameter of 1 mm is left. Valve 3 is inserted inside the ampoule,

made in the form of a disk of vacuum rubber with a thickness of 5 mm, cut into the inner diameter of the ampoule.

A sample of liquid or gas is introduced into the ampoule using a medical needle 4 through aperture 2 and valve 3. Previously, the ampoule can be evacuated using a needle connected to a vacuum system. To create excess pressure, a high pressure system is used with which the needle is connected by a long flexible metal capillary. After the sample is introduced and the corresponding pressure inside the ampoule is created, the needle can be easily removed from the valve. Pressure presses the valve against the opening and closes it, remaining fixed and equal to a predetermined time.

To change the sample, you need to re-insert the needle, gradually relieve pressure, pump out the sample of liquid or gas and replace it with a new one.

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A positive effect of using the cell of the proposed design arises when it is necessary to study samples with precisely specified concentrations (random error less than 0.1 May;%) and pressures (random error 0.01 MPa) of the components of the starting materials. Moreover, if the cell is used autonomously, i.e. disconnected from the high-pressure system, it can be rotated in the NMR sensor, which is necessary to record high-resolution spectra. If the cell remains connected to the high-pressure system, it becomes possible to maintain or change the pressure or concentration of the components of the starting materials in the same sample during the experiment without removing it from the sensor. In known variants of technical solutions, such features are not provided.

Tests of the proposed cell in a hydraulic press showed that when

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in the dimensions mentioned above, it easily withstands internal pressures of up to 15.0 MPa. Individual specimens withstand up to 25 MPa.

Experience with such cells indicates their high reliability and effectiveness.

Claims (1)

The claims A cell for NMR measurements in liquids and gases under pressure, which is a cylindrical quartz ampoule, characterized in that, in order to expand the functionality of NMR spectrometers by controlling the pressure and concentration of substances during the experiment, as well as simplifying the preparation process samples, in one of the ends of the ampoule left a hole to which from the inside there is a valve made in the form of a disk with a diameter corresponding to the inner diameter of the ampoule.