JPS6324436Y2 - - Google Patents

Description

[Detailed description of the invention] The present invention relates to a double sample tube used in nuclear magnetic resonance absorption (hereinafter abbreviated as NMR) experiments.

In NMR spectrometers, dual sample tubes have been published for a long time, in which the deuterated solvent and measurement sample liquid are placed in separate sample tubes, and both liquids are simultaneously placed in the spectrometer to measure the spectrum. FIG. 1 is a longitudinal sectional view showing an example of a conventional double sample tube. In the figure, 1 is an outer tube made of a glass tube with a bottom, and 2 is an inner stopper attached to the upper part of the outer tube 1. This inner plug 2 is made of Teflon (registered trademark name, the same applies hereinafter) or the like,
A through hole is drilled in its central axis. Reference numeral 3 denotes an inner tube made of a glass tube with a bottom, which is inserted into the through hole of the inner stopper 2 and disposed within the outer tube 1. A bottom plug 4 is disposed in the bottom of the outer tube 1 to support the bottom of the inner tube 3, and is made of Teflon or the like similarly to the inner tube 2.

With a double sample tube configured in this way, for example, the inner tube 3 is filled with a deuterated solvent and the outer tube 1 is filled with a sample liquid to be measured, which is then attached to the spinner of an NMR spectrometer and measured to obtain an NMR spectrum pattern. It's something you get. During measurement, if this double sample tube is not installed symmetrically with respect to the rotation axis, or if the inner tube 3 and outer tube 1 are not placed coaxially, spinning will occur on both sides of the NMR spectrum. Side bands (hereinafter abbreviated as SSB) occur, making analysis of NMR spectra difficult.

In recent years, as NMR using superconducting magnets has come into use, noise, which had low sensitivity and could be ignored in practical terms with older NMR spectrometers, has become clearly observed. This made it impossible to conduct good experiments. Furthermore, the cost of the deuterated solvent consumed in large-bore probes has increased significantly, and the economic burden has also increased significantly. Furthermore, since the inner tube is supported by inner and bottom plugs made of Teflon or other materials with low elasticity, it is difficult to secure the inner tube safely, and NMR signals are often generated, which interferes with proper measurements. It had various drawbacks.

The present invention was developed with this point in mind, and allows for extremely easy alignment of the inner and outer tubes, and does not cause misalignment even when rotated by a spinner.
The purpose is to provide a dual sample tube for NMR spectrometers, which consists of a cylindrical tube with a bottom made of non-magnetic material, with an outer tube formed in a conical shape whose bottom part shares a common central axis, and an outer tube made of an elastic material. It consists of a stopper that has concentric and accurately positioned through holes and is attached to the opening of the outer tube, and a bottomed cylindrical tube made of a non-magnetic material and has a hemispherical bottom. It is characterized in that it comprises an inner tube which is arranged so as to be in contact with the conical inner bottom of the outer tube, and whose upper end is supported by the through hole of the stopper.

An example of the implementation of the double sample tube for NMR spectrometer according to the present invention will be described below with reference to FIG.

FIG. 2 is a longitudinal sectional view showing an embodiment of the present invention. In the figure, reference numeral 11 denotes an outer tube, which is formed of a bottomed glass tube like the conventional one. The bottom portion 12 of the outer tube 11 is formed into a conical shape whose central axis is common to the central axis of the outer tube 11.
Reference numeral 13 denotes a stopper made of an elastic material such as silicone rubber, and a concentric through-hole that is accurately positioned is bored in the center thereof. Similarly to the conventional one, the inner tube 14 has a hemispherical bottom 15, and is inserted into the through hole of the stopper 13.
At this time, the inner tube 14 has its bottom 15 connected to the outer tube 1.
It is inserted until it touches the conical bottom 12 of 1.

The double sample tube configured in this way has an inner tube 14
However, since its upper part is supported by a concentrically precisely positioned through hole of the stopper 13, and the hemispherical bottom part 15 is supported in contact with the conical slope of the outer tube 11, the bottom part is particularly Not only can the outer tube 11 and the inner tube 14 be aligned extremely easily without the need for positioning devices such as stoppers, but the inner tube 14 is firmly supported at two locations, upper and lower. Therefore, even if it is attached to a spinner and rotated, there will be no axis misalignment.

Although the present invention has been described above according to the illustrated embodiment, it goes without saying that the present invention is not limited to this. For example, the conical shape of the bottom portion 15 of the outer tube 14 is not limited to a simple conical shape as shown in FIG. 2, but may also be a combination of two conical shapes as shown in FIG. 3, or a truncated conical shape. This includes Yon.

The same applies to the material of the stopper 13, and the material is not particularly selected as long as it has appropriate elasticity. For example, if heat sterilization is performed with the stopper 13 still in place, using a material that is breathable to the extent that it does not allow bacteria to pass through will prevent the stopper 13 from coming off due to air expansion during heating. It can be prevented. Furthermore, although the inner tube 14 is exemplified as having an open top end, it may be of a closed type in which an appropriate amount of deuterated solvent is injected and the top end is also sealed.

As described above, according to the double sample tube for NMR spectrometer according to the present invention, alignment with the outer tube is extremely easy without the need for special equipment, no matter what the outer diameter of the inner tube. Not only is this possible, but the head of the inner tube is supported by a plug made of elastic material such as silicone rubber, so
It can be safely and firmly attached without damaging the outer tube, and it can maintain a stable state as a whole even when attached to a spinner and rotated.
Analysis of NMR spectra becomes easier due to the significant reduction in SSB.

[Brief explanation of drawings]

FIG. 1 is a vertical cross-sectional view showing an example of a conventional double sample tube, and FIG. 2 is a vertical cross-sectional view showing an example of the present invention.
FIG. 3 is a longitudinal cross-sectional view of a main part showing another embodiment of the present invention. 1, 11... Outer pipe, 2... Inner stopper, 3, 14...
Inner tube, 4...bottom plug, 12, 15...bottom, 13...
…plug.

Claims (1)

[Scope of utility model registration request] It consists of a cylindrical tube with a bottom made of non-magnetic material, and has an outer tube formed in a conical shape whose bottom part shares a common central axis, and a through hole made of an elastic material and accurately positioned concentrically. , consisting of a plug attached to the opening of the outer tube and a bottomed cylindrical tube made of a non-magnetic material and having a hemispherical bottom, the bottom of which is arranged so as to be in contact with the conical inner bottom of the outer tube; A double sample tube for a nuclear magnetic resonance absorption spectrometer, comprising an inner tube whose upper end is supported by the through hole of the stopper.