WO2004063093A1 - 核スピン偏極キセノンガスの製造方法及び製造装置 - Google Patents
核スピン偏極キセノンガスの製造方法及び製造装置 Download PDFInfo
- Publication number
- WO2004063093A1 WO2004063093A1 PCT/JP2004/000093 JP2004000093W WO2004063093A1 WO 2004063093 A1 WO2004063093 A1 WO 2004063093A1 JP 2004000093 W JP2004000093 W JP 2004000093W WO 2004063093 A1 WO2004063093 A1 WO 2004063093A1
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- WO
- WIPO (PCT)
- Prior art keywords
- rubidium
- xenon
- glass cell
- pipe
- gas
- Prior art date
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Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/06—Nuclear magnetic resonance [NMR] contrast preparations; Magnetic resonance imaging [MRI] contrast preparations
- A61K49/18—Nuclear magnetic resonance [NMR] contrast preparations; Magnetic resonance imaging [MRI] contrast preparations characterised by a special physical form, e.g. emulsions, microcapsules, liposomes
- A61K49/1806—Suspensions, emulsions, colloids, dispersions
- A61K49/1815—Suspensions, emulsions, colloids, dispersions compo-inhalant, e.g. breath tests
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B23/00—Noble gases; Compounds thereof
- C01B23/001—Purification or separation processes of noble gases
- C01B23/0036—Physical processing only
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0029—Obtaining noble gases
- C01B2210/0037—Xenon
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0043—Impurity removed
Definitions
- the present invention relates to a method and an apparatus for producing a nuclear spin-polarized xenon gas. More specifically, the present invention relates to a nuclear spin polarization capable of continuously producing a high concentration of polarized nuclear spins useful for an NMR / MRI apparatus. The present invention relates to a method and an apparatus for producing xenon gas. '
- polarized means that the distribution of the number of spins occupying the nuclear energy level of the nucleus corresponding to the orientation state with respect to the main static magnetic field is extremely deviated from that at thermal equilibrium. That means.
- the rare gas having a state of the polarized is xenon one 1 2 9 (1 2 9 X e), helium one 3 (9 H e) Single with nuclear spin of the spin quantum number 1 Z 2, such as
- a rare gas containing atomic molecules with an alkali metal vapor such as rubidium or cesium, electrons at the ground state level of rubidium or the like are excited by light absorption.
- a conventional polarized rare gas production apparatus encloses a mixed gas of a rare gas and an alkali metal vapor in a photoreaction vessel and irradiates it with excitation light and applies a magnetic field.
- I-3 as a neutron polarizer
- 1% xenon is mixed with a buffer gas of a hemisphere of about 10 atmospheres, introduced into a cylindrical glass container, irradiated, polarized, and guided into a dewar cooled by liquid nitrogen from the gas outlet of the container.
- polarized xenon is separated into solids and separated, and the remaining helium gas is discharged from the vent line (for example, B. Driehuys, GD Gates, E. Miron, K. Sauer, DK Walter and W. Happer, Appl. Phys, Lett. 69, 1668 (1996)).
- the operation for increasing the polarization is performed by irradiating a laser beam while keeping a rare gas or the like in the photoreaction vessel.
- the polarization rate has increased, cool to room temperature and use it as a neutron polarizer, or heat the polarized xenon-129 once solid-separated in the duct once again to gasify it, and use another vessel. And used for NMR and other measurements.
- xenon is diluted to a concentration of, for example, about 2% xenon in helium to polarize the gas, and the generated gas containing xenon is frozen with liquid nitrogen and heated. Since only xenon was taken out to produce high-concentration xenon gas, there was a problem of extremely low work efficiency.
- conventional devices that retain and polarize gases etc. cannot continuously generate polarized rare gases, so take out the polarized gas to another container and transport it to an NMR system etc. Therefore, there was a problem that it took time and during that time the polarization rate decreased.
- the present invention has been made in view of such a point, and a manufacturing method and a manufacturing method capable of obtaining a high-concentration polarized xenon gas without freezing and continuously generating the polarized xenon gas. It is intended to provide a device.
- Another object of the present invention is to provide a method and an apparatus for manufacturing a glass cell in which metal rubidium and xenon gas used in the above-described method and apparatus are solidified and sealed in the absence of oxygen.
- the production method according to claim 1 of the present invention comprises heating a glass cell in which solid norevidium and solid xenon are sealed under reduced pressure in the absence of oxygen to obtain gas xenon and gas-liquid mixed rubidium, It is characterized by applying a magnetic field to irradiate laser light.
- the absence of oxygen is to prevent solid rubidium from being oxidized, and the presence of a trace amount of oxygen that does not hinder the reaction because solid rubidium is oxidized is allowed.
- the xenon gas supply device side is set as the primary side via the first air operated valve, the xenon gas introduction side of the glass cell is set as the secondary side, and the evacuation of the primary side piping is performed. It is preferable that the pressurized standing with nitrogen gas is automatically repeated three times or more.
- the primary side pipe, the secondary side pipe, and the primary side pipe are evacuated to the primary xenon gas outlet side valve communicating with the polarized xenon gas outlet side valve via the second air operated valve. It is preferable to automatically repeat the pressurizing and releasing by nitrogen gas in the side piping at least three times.
- a chamber accommodating rubidium sealed in a glass container is connected to the glass cell so as to communicate with a pipe, and the pipe is evacuated with a vacuum generator.
- the enclosed glass container is cracked, and the metal rubidium, the pipe and the glass cell are heated, gaseous rubidium is present in the pipe and the glass cell, and then the glass cell is cooled, and the metal rubidium is solidified in the cooled part.
- the glass cell is sealed by introducing xenon gas into the glass cell, and the glass cell is cooled to solidify xenon in the glass cell.
- the production apparatus of the present invention comprises means for heating a glass cell in which solid rubidium and solid xenon are sealed in a reduced pressure state in the absence of oxygen to form gaseous xenon and gas-liquid mixed rubidium, and applying a magnetic field to the glass cell. And a means for irradiating a laser beam.
- a means for introducing the xenon gas while taking out the generated nuclear spin-polarized xenon gas and a pressure adjusting means for controlling the operation so that the pressure does not drop.
- a xenon gas supply device side is used as a primary pipe through a first air operated valve, a secondary pipe is used up to a valve for introducing xenon gas into a glass cell, and a second air operated valve is provided in the primary pipe.
- One of the branched pipes is connected to a vacuum generator, the other is connected to a polarized xenon gas outlet side valve of the glass cell, and the primary pipe is connected to a glass cell. It is preferable to provide pressure adjusting means for adjusting the pressure to be introduced.
- An apparatus for producing a glass cell comprises: a pipe connecting a chamber containing rubidium sealed in a glass container and the glass cell so as to communicate with each other; a means for emptying the pipe; and a rubidium. It is characterized by comprising means for breaking the enclosed glass, means for heating metal rubidium, piping and glass cells, and means for cooling the glass cells and depositing metal rubidium in the cooled part.
- the present invention provides that a highly concentrated xenon gas can be obtained without freezing by sealing and heating xenon in a glass cell to which metal rubidium is adhered and irradiating the laser beam. It is a summary.
- FIG. 1 is a schematic sectional view showing an apparatus for producing a glass cell in which rubidium and xenon are sealed according to the present invention.
- FIG. 2 is a cross-sectional view showing a state in which the glass cell is closed and sealed after enclosing rubidium and xenon.
- FIG. 3 is a configuration diagram showing one embodiment of the manufacturing apparatus of the present invention.
- Fig. 1 shows a method of manufacturing a glass cell enclosing rubidium and xenon (manufacturing equipment).
- Metal rubidium wrapped in glass (1) A piping (4) connecting the chamber (2) and the glass cell (3) is connected to a vacuum pump 5 and the xenon gas supply line 6 are connected.
- Rubidium is oxidized into rubidium oxide when it comes into contact with air, so it is enclosed in glass as described above when purchased from a manufacturer. In this state, the pulp Vxe and the valves V1 and V2 are closed.
- valve Vp If the valve Vp is opened and the vacuum pump 5 is evacuated with the valve VXe closed, the air in the pipe 4 and the glass cell 3 is exhausted. If the glass enclosing rubidium is broken in this state, the metal rubidium will not be oxidized because it will be present in a vacuum. A magnet wrapped in glass is also enclosed in the room 2 for metal rubidium 1, which is moved by a magnet from outside to break the glass against metal rubidium 1 wrapped in glass.
- the heating temperature should be higher than the melting point of rubidium (about 40 ° C) and a temperature at which rubidium is in a gas-liquid mixed state in which a liquid and a gas corresponding to the vapor pressure at that temperature exist at a high concentration.
- the temperature is preferably from 130 to 180 ° C, and particularly preferably around 150 ° C.
- this glass cell When this glass cell is used and is configured as shown in FIG. 3 and the temperature of the glass cell 3 is raised to a temperature of preferably 50 to 180 ° C., particularly preferably around 120 ° C., the glass In the cell, xenon gas and gas-liquid mixed rubidium are formed. This state If you apply a magnetic field and irradiate the laser, it takes tens of minutes
- valves V2 and V3 are opened to collect the polarized xenon gas with the polarized xenon gas sampling cylinder 9, and at the same time, the pulp V1 is opened to prevent the pressure from dropping and the auto pressure regulator ( (APC) Introduce xenon gas while adjusting the pressure at 10.
- APC auto pressure regulator
- the polarized xenon gas in the glass cell 3 is taken out, the pressure drops and the air flows backward, so xenon gas whose pressure is controlled as described above is introduced.
- the air operated valves AV6, AVI and AV3 and the valves VI, V2 and V3 in FIG. 3 are open.
- valves V1 and V2 are closed, and the entire glass cell 3 is cooled with liquid nitrogen to solidify xenon. Then, the glass cell 3 is heated to produce polarized xenon gas by the same operation as described above. In this way, the catalyst can be continuously and repeatedly produced until rubidium in the catalyst is eliminated.
- xenon gas from the xenon cylinder 11 passes through the air operated valve (AV1), the auto pressure regulator (APC) 10 and the first air operated valve (AV3), and passes through the valve V 1 of the glass cell 3.
- the pressure for taking out the polarized xenon gas is about 1.5 atm. Therefore, the pressure of the xenon gas is adjusted to about 1.5 atm by the APC 10.
- the valves VI to V4 are composed of glass bulbs, because the polarized xenon gas comes into contact with the bulb, and if the glass is not used, the polarized xenon gas returns to the xenon gas. Therefore, the other part of the pipe where the polarized xenon gas comes into contact is also made of glass (Pyrex glass).
- Nitrogen gas and xenon gas are respectively reduced to a pressure of about 1.5 atm by pressure reducing valves (REG2 and REG1).
- Air is mixed in when replacing the cylinder and when replacing the glass cell. In this case, air is prevented from entering the glass cell as follows.
- air enters the piping between the cylinder's main valve 13 and the air operated pulp (AV1) and air operated pulp (AV6).
- To remove this air turn on the vacuum pump (P) 15 and open the air operated valve (AV 1), air operated valve (AV 2), and second air operated pulp (AV 4), and remove the inside of the primary side piping.
- Vacuum and pressure transmitter It is left for a predetermined time while detecting the degree of decompression with the printer (PT1).
- the xenon gas supply device side is the primary side via the first air operated valve (AV 3), and the xenon gas introduction side of the glass cell is the secondary side.
- valve V4 and the second air operated valve (AV4) control the communication between the downstream side pipe and the vacuum pump), and evacuate the inside of the pipe of the aeration section.
- first air operated valve (AV 3) connecting the primary and secondary piping and the valve from both cylinders to the first air operated pulp (AV 3) to open the primary piping and the secondary piping.
- the steps of opening the first air operated valve and the second air operated pulp, evacuating the air in the same manner as described above, and leaving it under pressure are repeated.
- oxygen can be prevented from being mixed into the glass cell.
- a pressure transmitter (PT 2) is provided in the secondary side piping, the pressure is detected and the evacuation and pressurization for a predetermined time are performed while detecting the pressure.
- the air operated valve (AV 5) in FIG. 3 is pulp for releasing gas when the primary pipe is pressurized, but is not used in the above operation.
- nitrogen and xenon gas are supplied from a cylinder, but this may be another known gas supply device.
- a polarized xenon gas can be obtained by reacting at a high concentration of xenon gas of 80 to 100% (remainder is nitrogen gas). Therefore, a treatment such as solidification after polarization is performed.
- a high-density polarized xenon gas can be obtained without any problem.
- by performing evacuation and leaving the pipe under pressure many times it is possible to prevent air from entering the glass cell.
- high-concentration xenon gas is used as described above, according to the present invention, high-concentration polarized xenon gas can be produced using high-concentration xenon gas, so that it is possible to eliminate the trouble of freezing and concentrating after production as in the conventional method. it can.
- the inside of the pipe can be sufficiently purged, so that air can be prevented from entering the reaction glass cell and the life of the rubidium catalyst can be extended. Can be.
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Abstract
Description
Claims
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US10/541,704 US8217293B2 (en) | 2003-01-10 | 2004-01-09 | Process and system for producing nuclear spin polarized xenon gas |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2003-004304 | 2003-01-10 | ||
JP2003004304A JP3998243B2 (ja) | 2003-01-10 | 2003-01-10 | 核スピン偏極キセノンガスの製造方法及び製造装置 |
Publications (1)
Publication Number | Publication Date |
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WO2004063093A1 true WO2004063093A1 (ja) | 2004-07-29 |
Family
ID=32708946
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/JP2004/000093 WO2004063093A1 (ja) | 2003-01-10 | 2004-01-09 | 核スピン偏極キセノンガスの製造方法及び製造装置 |
Country Status (3)
Country | Link |
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US (1) | US8217293B2 (ja) |
JP (1) | JP3998243B2 (ja) |
WO (1) | WO2004063093A1 (ja) |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4817317B2 (ja) * | 2006-11-24 | 2011-11-16 | 独立行政法人産業技術総合研究所 | 核スピン偏極希ガスの製造装置と核磁気共鳴分光装置並びに核磁気共鳴イメージング装置 |
WO2009143368A2 (en) * | 2008-05-23 | 2009-11-26 | University Of Utah | Non-cryogenic storage cell for hyperpolarized 129xe |
JP5191543B2 (ja) | 2008-08-01 | 2013-05-08 | 国立大学法人大阪大学 | 偏極キセノンガスの濃縮方法、偏極キセノンガスの製造供給装置及びmriシステム |
US8071019B2 (en) | 2008-10-31 | 2011-12-06 | Honeywell International Inc. | Methods for introduction of a reactive material into a vacuum chamber |
DE102020206031A1 (de) | 2020-05-13 | 2021-11-18 | Robert Bosch Gesellschaft mit beschränkter Haftung | Vorrichtung zum Befüllen einer Dampfzelleneinrichtung mit einem Gas, Verfahren zum Herstellen einer mit einem Gas befüllten Dampfzelleneinrichtung, und Dampfzelleneinrichtung |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5545396A (en) * | 1994-04-08 | 1996-08-13 | The Research Foundation Of State University Of New York | Magnetic resonance imaging using hyperpolarized noble gases |
JPH11248809A (ja) * | 1998-03-03 | 1999-09-17 | Agency Of Ind Science & Technol | 偏極希ガスの製造装置を有する核磁気共鳴検出装置並びにその装置を用いる核磁気共鳴測定方法 |
Family Cites Families (17)
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US2712384A (en) * | 1952-09-27 | 1955-07-05 | Du Pont | Handling metallic sodium |
US5039500A (en) * | 1988-11-18 | 1991-08-13 | Kyodo Oxygen Co., Ltd. | Process for producing xenon |
US5617860A (en) * | 1995-06-07 | 1997-04-08 | Smithsonian Astrophysical Observatory | Method and system for producing polarized 129 Xe gas |
IL126347A (en) * | 1996-03-29 | 2003-11-23 | Lawrence Berkeley National Lab | Enhancement of nmr and mri in the presence of hyperpolarized noble gases |
US5642625A (en) * | 1996-03-29 | 1997-07-01 | The Trustees Of Princeton University | High volume hyperpolarizer for spin-polarized noble gas |
US5809801A (en) * | 1996-03-29 | 1998-09-22 | The Trustees Of Princeton University | Cryogenic accumulator for spin-polarized xenon-129 |
US5934103A (en) * | 1997-04-22 | 1999-08-10 | Northrop Grumman Corporation | Method and apparatus for production of spin-polarized medical-grade xenon 129 gas by laser optical pumping |
US6085743A (en) * | 1997-05-30 | 2000-07-11 | The Regent Of The University Of Michigan | Polarized gas delivery system/method |
US6318092B1 (en) * | 1997-08-18 | 2001-11-20 | The Trustees Of Princeton University | Alkali metal hybrid spin-exchange optical pumping |
US6079213A (en) * | 1997-12-12 | 2000-06-27 | Magnetic Imaging Technologies Incorporated | Methods of collecting, thawing, and extending the useful life of polarized gases and associated accumulators and heating jackets |
US6523356B2 (en) * | 1998-09-30 | 2003-02-25 | Medi-Physics, Inc. | Meted hyperpolarized noble gas dispensing methods and associated devices |
US6125654A (en) * | 1998-10-16 | 2000-10-03 | Syracuse University | Bulk production and usage of hyperpolarized 129 Xenon |
DE19937566C2 (de) * | 1999-08-09 | 2001-06-28 | Forschungszentrum Juelich Gmbh | Hochdruckpolarisator für Edelgase und Verfahren zum Betreiben des Polarisators |
DE10000675C2 (de) * | 2000-01-11 | 2001-11-15 | Otten Ernst Wilhelm | Lineardurchführung, Vorrichtung und Verfahren zur hochproduktiven Erzeugung von hoch kernspinpolarisiertem Helium-3 Gas |
US7287390B2 (en) * | 2001-10-22 | 2007-10-30 | Medi-Physics, Inc. | Optical pumping modules, polarized gas blending and dispensing systems, and automated polarized gas distribution systems and related devices and methods |
JP4169122B2 (ja) * | 2002-02-26 | 2008-10-22 | 独立行政法人産業技術総合研究所 | 核スピン偏極希ガスの製造装置とこれを用いた偏極希ガスの製造方法 |
NO20025124D0 (no) * | 2002-10-25 | 2002-10-25 | Amersham Health As | Metode |
-
2003
- 2003-01-10 JP JP2003004304A patent/JP3998243B2/ja not_active Expired - Fee Related
-
2004
- 2004-01-09 US US10/541,704 patent/US8217293B2/en active Active
- 2004-01-09 WO PCT/JP2004/000093 patent/WO2004063093A1/ja active Application Filing
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5545396A (en) * | 1994-04-08 | 1996-08-13 | The Research Foundation Of State University Of New York | Magnetic resonance imaging using hyperpolarized noble gases |
JPH11248809A (ja) * | 1998-03-03 | 1999-09-17 | Agency Of Ind Science & Technol | 偏極希ガスの製造装置を有する核磁気共鳴検出装置並びにその装置を用いる核磁気共鳴測定方法 |
Non-Patent Citations (1)
Title |
---|
RAFTERY D. ET AL: "High-Field NMR of Adsorbed Xenon Polarized by Laser Pumping", PHYSICAL REVIEW LETTERS, vol. 66, no. 5, 1991, pages 584 - 587, XP002979367 * |
Also Published As
Publication number | Publication date |
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JP2004262668A (ja) | 2004-09-24 |
US20060083789A1 (en) | 2006-04-20 |
JP3998243B2 (ja) | 2007-10-24 |
US8217293B2 (en) | 2012-07-10 |
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