JP3338602B2 - Spinner for high-resolution solid-state NMR measurement - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a solid-state high-resolution NM.
More specifically, the present invention relates to a spinner for R measurement, and more particularly to a spinner for high-resolution solid-state NMR measurement which prevents the leakage of a liquid substance during measurement of a sample containing the liquid substance during solid-state high-resolution NMR measurement, thereby facilitating the above measurement. About.

[0002]

2. Description of the Related Art When measuring a solid high-resolution NMR of a sample, a spinner for solid-state high-resolution NMR measurement which is accommodated in a sample and mounted on a solid-state high-resolution NMR measuring instrument is generally shown in FIG. A spinner as shown, that is, a cylindrical main body 1 having an opening at one end, and a lid 2 fitted into the opening of the cylindrical main body 1. There is known a spinner to which an O-ring 4 is attached so that the sample accommodated in the hollow portion 11 does not leak from the hollow portion 11 of the tubular main body 1. The solid-state high-resolution NMR measurement of the sample is performed by accommodating the sample in the solid-state high-resolution NMR measurement spinner, attaching the sample to the solid-state high-resolution NMR measuring instrument, and rotating at high speed. .

[0003]

However, oil-containing samples, such as cosmetics such as foundations, foods such as fried confections, and biological samples containing water and oil, are added to the above-mentioned conventional solid-state high-resolution NMR spinner. When a solid-state high-resolution NMR is to be measured by accommodating a sample containing a liquid material, the liquid material is centrifugally applied along the inner surface of the cylindrical body 1 during the measurement. , But the liquid material that has flowed
There is a problem that it is difficult to be sealed by the ring 4 and oozes out between the cylindrical main body 1 and the lid 2 to contaminate the cylindrical main body 1, the lid 2 and the solid high-resolution NMR measuring instrument. there were. In addition, the oozed liquid material makes it difficult for the solid high-resolution NMR measuring device to operate normally, and furthermore, there is even a risk that the solid high-resolution NMR measuring device may be burned out by friction during high-speed rotation. Further, the operator has to work to clean the contaminated solid high-resolution NMR measurement device after each measurement.

Accordingly, it is an object of the present invention to provide a solid-state high-resolution NMR spectrometer which can easily perform the above-mentioned measurement by preventing the liquid substance from leaking during the solid-state high-resolution NMR measurement of a sample containing the liquid substance. A spinner.

[0005]

The present invention comprises a cylindrical main body 1 having an opening at one end and a lid 2 fitted into the opening of the cylindrical main body 1. When performing the measurement, the sample is accommodated, and a solid high-resolution NMR measurement spinner used by being attached to a solid high-resolution NMR measuring instrument is provided with an insert 3 inserted into the hollow portion 11 of the cylindrical main body 1. The insert 3 is made of an elastic material, is formed of a hollow body with a bottom provided with a sample container 32 having an opening 31 at one end, and a sample containing a liquid substance in the sample container 32 of the insert 3. After housing the S, the insert 3 is inserted into the hollow portion 11 of the tubular main body 1 from the opening 31 side, the lid 2 is fitted into the opening of the cylindrical main body 1, and the solid Be attached to a resolution NMR measuring instrument By providing a high-resolution solid-state NMR measurement spinner, characterized it is obtained by achieving the above object.

[0006]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments of the spinner for solid-state high-resolution NMR measurement according to the present invention will be specifically described below with reference to the drawings. FIG. 1 is a longitudinal sectional view showing an embodiment of the solid state high-resolution NMR measurement spinner of the present invention, FIG. 2 is a perspective view of an insert in the embodiment shown in FIG.
FIG. 3 is a longitudinal sectional view showing one production form of the insert shown in FIG. 2 together with a mold for producing an insert.

A spinner for solid-state high-resolution NMR measurement according to this embodiment includes a cylindrical tubular main body 1 having an opening at one end;
A lid 2 fitted into the opening of the tubular main body 1;
When a sample is measured for solid-state high-resolution NMR, the sample is accommodated and used by being attached to a solid-state high-resolution NMR measuring instrument. The above configuration is the same as that of the conventional solid-state high-resolution NMR measurement spinner.

Thus, the solid-state high-resolution NMR of this embodiment
The measurement spinner includes an insert 3 that is inserted into the hollow portion 11 of the tubular main body 1.
After the sample S containing a liquid substance is accommodated in the sample accommodating portion 32 of the insert 3, the sample S is made of an elastic material and has a bottomed hollow body provided with a sample accommodating portion 32 having an opening 31 at one end. The insert 3 is inserted into the hollow portion 11 of the tubular main body 1 from the opening 31 side, and
The lid 2 is fitted to the opening of the solid-state high-resolution NMR.
It is designed to be attached to a measuring instrument.

More specifically, as shown in FIGS. 1 and 2, the bottomed hollow body 3 as the insert 3 is inserted into a hollow portion 11 of the cylindrical main body 1 as shown in FIGS. When the cover 2 is fitted into the opening of the cylindrical body 1, the outer surface of the cylindrical body 1 is formed into a cylindrical shape having such a size as to be in close contact with the inner surface of the cylindrical body 1. The height is the same as the height of the hollow portion 11 of the tubular main body 1. The hollow portion 32 of the bottomed hollow body 3 serving as the sample storage section 32 is formed so that the thickness of the bottomed hollow body 3 is as small as possible, and is preferably 2 mm or less, and more preferably 0 mm or less. .5m
m or less.

The elastic material forming the insert 3 is made of silicone rubber, and the silicone rubber is made of a curable silicone resin.
This material (silicone rubber) has no effect on the solid-state high-resolution NMR measurement of the sample S and has rubber elasticity. The elastic material may be any material that does not affect the measurement and has rubber elasticity, and may be any other material, for example, fluorine rubber or any rubber material such as isoprene rubber in measurement other than carbon. It can also be formed.

In using the spinner for solid-state high-resolution NMR measurement of the present embodiment configured as described above, the sample S containing the liquid substance is accommodated in the sample accommodating portion 32 of the insert 3, and then the sample S shown in FIG. As shown, the insert 3
Is inserted into the hollow portion 11 of the tubular body 1 from the opening 31 side so that the opening 31 is sealed by the bottom plate 12 of the tubular body 1, and the sample S containing the liquid substance is It is sealed in the sample container 32. The outer surface of the insert 3 is in close contact with the inner surface of the tubular body 1 when the insert 3 is inserted into the hollow portion 11 of the tubular body 1 as shown in FIG. . Then, the cylindrical main body 1
The lid 2 is fitted to the opening 2 by screwing the convex portion 21 thereof.
By mounting the spinner for high-resolution solid-state NMR measurement of the present embodiment on the above-described high-resolution solid-state NMR measurement device, high-resolution solid-state NMR of the sample S containing the liquid substance is measured.

When the solid-state high-resolution NMR measurement of the sample S containing the liquid substance is performed by the solid-state high-resolution NMR measurement spinner of the present embodiment, the outer surface of the insert 3 is centrifugally moved by the centrifugal force. Since the liquid substance is pressed against the inner surface of the cylindrical main body 1 and completely adheres to the inner surface of the cylindrical main body 1, the liquid substance does not seep out from between the cylindrical main body 1 and the lid 2, and the solid height does not increase. The above measurement can be easily performed without contamination of the resolution NMR measuring instrument and the like.

It should be noted that the present invention is not limited to the above-described embodiment, but may be made within the scope of the present invention.
Its size, shape, etc. can be changed as appropriate. For example, easily without dropping the sample from the opening 31,
A lid or the like may be provided at the opening 31 of the insert 3 so that the insert 3 can be inserted into the hollow portion 11 of the tubular main body 1. Further, when the outer surface of the insert 3 is deformed by centrifugal force, the thickness of the insert 3 is set to 0.
It is preferable to set to about 1 to 2 mm and to set the initial Young's modulus of the insert 3 to 10 ⁶ to 10 ⁷ dyne / cm ² . Furthermore, in the above-described embodiment, the height of the insert 3 is the same as the height of the hollow portion 11 of the tubular main body 1 when the lid 2 is fitted into the opening of the tubular main body 1, The cylindrical body 1 when the lid 2 is fitted into the opening of the cylindrical body 1
May be lower than the height of the hollow portion 11. Further, the cylindrical main body 1 and the lid 2 may be appropriately used conventional ones, and the insert 3 may be formed in a shape suitable for it.

Next, the insert 3 of the present embodiment described above
A preferred production method of the invention will be described. That is, first,
A liquid silicone material is obtained by kneading a dental silicone resin (GC Exa Fine Injection Type [GC Co., Ltd.]) as a curable silicone resin and a curing agent as a catalyst.

Next, after the mixed liquid material is poured into the female mold 51 of the insert manufacturing formwork 5 as shown in FIG. 3, the male mold 52 is fitted, and the state is left for about 10 minutes. Thus, the liquid mixture is cured to obtain a cured product 53 of the liquid mixture. Thereafter, the cured product 53 is released from the insert manufacturing mold 5 and the burr 53 of the cured product 53 is removed.
The insert 3 is obtained by cutting a and cutting the height h to a predetermined height. It is preferable that the insert manufacturing mold 5 be formed of a fluororesin, particularly Teflon (registered trademark) in order to easily remove the cured product 53 of the mixed liquid material.

[0016]

According to the spinner for solid-state high-resolution NMR measurement of the present invention, leakage of a liquid substance during the measurement of a sample containing the liquid substance during solid-state high-resolution NMR measurement can be prevented.
The above measurement can be easily performed.

[0017]

[Brief description of the drawings]

FIG. 1 is a longitudinal sectional view showing an embodiment of a spinner for solid-state high-resolution NMR measurement of the present invention.

FIG. 2 is a perspective view of the insert in the embodiment shown in FIG.

FIG. 3 is a longitudinal sectional view showing one production form of the insert shown in FIG. 2 together with a mold for producing an insert.

FIG. 4 is a longitudinal sectional view showing a conventional solid-state high-resolution NMR measurement spinner with an O-ring.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Cylindrical main body 11 Hollow part of a cylindrical main body 2 Lid 3 Insert 31 Opening 32 Sample accommodating part S Sample containing a liquid material

Claims (3)

(57) [Claims] 1. A cylindrical body 1 having an opening at one end, and a lid 2 fitted into the opening of the cylindrical body 1. When the sample is measured for solid-state high-resolution NMR, the sample is removed. Contain
In a solid high-resolution NMR measurement spinner used by being attached to a solid high-resolution NMR measurement device, an insert 3 inserted into the hollow portion 11 of the cylindrical main body 1
The insert 3 is made of an elastic material, and is formed of a hollow body with a bottom provided with a sample storage portion 32 having an opening 31 at one end. A liquid substance is placed in the sample storage portion 32 of the insert 3. After accommodating the contained sample S, the insert 3 is inserted into the hollow portion 11 of the tubular main body 1 from the opening 31 side, and the lid 2 is fitted into the opening of the cylindrical main body 1, A spinner for solid-state high-resolution NMR measurement, which is mounted on the solid-state high-resolution NMR measurement device. 2. The spinner for high-resolution solid-state NMR measurement according to claim 1, wherein the elastic material is made of silicone rubber and / or fluorine-based rubber. 3. The spinner for solid-state high-resolution NMR measurement according to claim 2, wherein the silicone rubber is obtained from a curable silicone resin as a raw material.