WO2003079034B1 - Flow-through cryogenic nmr probe - Google Patents

Flow-through cryogenic nmr probe

Info

Publication number
WO2003079034B1
WO2003079034B1 PCT/IB2003/002430 IB0302430W WO03079034B1 WO 2003079034 B1 WO2003079034 B1 WO 2003079034B1 IB 0302430 W IB0302430 W IB 0302430W WO 03079034 B1 WO03079034 B1 WO 03079034B1
Authority
WO
WIPO (PCT)
Prior art keywords
sample
sample cell
cell
coil
anyone
Prior art date
Application number
PCT/IB2003/002430
Other languages
French (fr)
Other versions
WO2003079034A2 (en
WO2003079034A3 (en
Inventor
Martin Hofmann
Manfred Spraul
Robert Eric Nast
Damon Leslie Harris
Original Assignee
Bruker Biospin Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Bruker Biospin Corp filed Critical Bruker Biospin Corp
Priority to EP03744486A priority Critical patent/EP1488247B1/en
Priority to DE60323068T priority patent/DE60323068D1/en
Publication of WO2003079034A2 publication Critical patent/WO2003079034A2/en
Publication of WO2003079034A3 publication Critical patent/WO2003079034A3/en
Publication of WO2003079034B1 publication Critical patent/WO2003079034B1/en

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00—Arrangements or instruments for measuring magnetic variables
    • G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
    • G01R33/28—Details of apparatus provided for in groups G01R33/44 - G01R33/64
    • G01R33/30—Sample handling arrangements, e.g. sample cells, spinning mechanisms
    • G01R33/307—Sample handling arrangements, e.g. sample cells, spinning mechanisms specially adapted for moving the sample relative to the MR system, e.g. spinning mechanisms, flow cells or means for positioning the sample inside a spectrometer
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00—Arrangements or instruments for measuring magnetic variables
    • G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
    • G01R33/28—Details of apparatus provided for in groups G01R33/44 - G01R33/64
    • G01R33/32—Excitation or detection systems, e.g. using radio frequency signals
    • G01R33/34—Constructional details, e.g. resonators, specially adapted to MR
    • G01R33/34015—Temperature-controlled RF coils
    • G01R33/34023—Superconducting RF coils
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00—Arrangements or instruments for measuring magnetic variables
    • G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
    • G01R33/28—Details of apparatus provided for in groups G01R33/44 - G01R33/64
    • G01R33/32—Excitation or detection systems, e.g. using radio frequency signals
    • G01R33/34—Constructional details, e.g. resonators, specially adapted to MR
    • G01R33/34092—RF coils specially adapted for NMR spectrometers

Landscapes

  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Magnetic Resonance Imaging Apparatus (AREA)
  • Investigating Or Analyzing Materials By The Use Of Magnetic Means (AREA)
  • Investigating Or Analyzing Materials Using Thermal Means (AREA)

Abstract

A nuclear magnetic resonance (NMR) spectroscopy probe has a sample cell into and out of which a room temperature liquid sample may be directed, The cell is surrounded by a radio frequency coil that is used to perform NMR measurements of the liquid sample, and which is maintained at cryogenic temperatures. The coil is separated from the sample cell by a thermally insulative boundary, such as a vacuum. The sample may enter the cell through an input path, and may exit through an output path. The input path, output path and sample cell may be surrounded by a sheath through which flows room temperature gas. The ends of the sample cell may be tapered to promote thorough flow through the cell, and flow diverters may be included in the sample cell adjacent to the input and output paths to force flow to the outer wall of the sample cell.

Claims

AMENDED CLAIMS[received by the International Bureau on 09 December 2003 (09.12.03); original claims 1-47 replaced by new claims 1-21 (4 pages)]
1. A cryogenically cooled probe apparatus for nuclear magnetic resonance spectroscopy, the apparatus comprising: a sample cell for containing a liquid sample, the sample cell being adapted to allow flow of the liquid sample into and out of the cell; an input path through which the liquid sample is directed to the sample cell and an output path through which the liquid sample may be removed from the cell; and a radio frequency (RF) coil surrounding the sample cell, the coil being maintained at cryogenic temperatures and being separated from the sample by a thermally insulative boundary.
2. An apparatus according to Claim 1 wherein the insulative boundary between the coil and the sample cell comprises a vacuum.
3. An apparatus according to Claim 1 or 2 wherein the insulative boundary is such that the temperature of the liquid sample, while in the sample cell, remains at approximately an ambient temperature surrounding the apparatus.
4. An apparatus according to anyone of the preceding claims further comprising a heat exchanger thermally coupled to the coil that maintains the coil at cryogenic temperatures.
5. An apparatus according to any one of the preceding claims wherein the sample cell is tapered outward adjacent to the input and output paths. 19
6. An apparatus according to Claim 5 further comprising at least one flow diverter in at least one tapered portion of the sample cell that forces flow of fluid toward an outer wall of the sample cell adjacent to the flow diverter.
7. An apparatus according to anyone of the preceding claims further comprising a sheath surrounding the input and output paths and the sample cell, within which may be contained a material that helps maintain the sample flowing through the paths at a relatively high temperature relative to the coil, wherein the relatively high temperature is preferably approximately equal to an ambient temperature surrounding the apparatus.
8. An apparatus according to Claim 7 wherein the material contained in the sheath flows from an input port to an output port.
9. An apparatus according to Claim 8 wherein the material is a gas approximately equal in temperature to an ambient temperature surrounding the apparatus, and wherein the gas flows through the sheath while the liquid sample is in the sample cell.
10. An apparatus according to Claim 9 wherein the input and output paths include a path through an outer casing surrounding the apparatus.
11. An apparatus according to anyone of claims 7 to 10 wherein an outer wall of the sheath separates the sample cell from a vacuum that functions, at least in part, as said insulative boundary.
12. An apparatus according to anyone of the preceding claims wherein the coil is maintained at a temperature of less than 40°K. 20
13. An apparatus according to anyone of the preceding claims wherein the sample cell resides permanently within a probe housing.
14. An apparatus according to anyone of the preceding claims wherein an outer wall of the sample cell separates the sample from a vacuum that functions, at least in part, as said insulative boundary.
15. An apparatus according to Claim 14 further comprising a coating on an outer surface of the sample cell outer wall, the coating providing thermal insulation to the sample cell and/or blocking thermal radiation from the sample cell.
16. An apparatus according to Claim 15 wherein the coating comprises an active heating element.
17. An apparatus according to anyone of the preceding claims further comprising a reference cell that resides adjacent to the sample cell, a reference material in the reference cell also being detectable by the RF coil.
18. An apparatus according to Claim 17 wherein the reference cell surrounds the sample cell.
19. An apparatus according to Claim 18 wherein the reference cell comprises a fluid path for a reference fluid that flows past an outer wall of the sample cell.
20. An apparatus according to Claim 18 wherein the reference fluid provides a thermal boundary that prevents heat loss from the sample cell. 21
21. A method of providing a nuclear magnetic resonance spectroscopic measurement of a liquid sample in particular using an apparatus according to anyone of the preceding claims, the method comprising: providing a sample cell for containing a liquid sample, the sample cell being adapted to allow flow of the liquid sample into and out of the cell; surrounding the sample cell with a radio frequency (RF) coil that is maintained at cryogenic temperatures and kept thermally separated from the sample cell by a thermally insulative boundary; directing flow of the sample into the sample cell and activating the coil to perform the desired measurement; and directing flow of the sample out of the sample cell.
PCT/IB2003/002430 2002-03-15 2003-03-13 Flow-through cryogenic nmr probe WO2003079034A2 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP03744486A EP1488247B1 (en) 2002-03-15 2003-03-13 Flow-through cryogenic nmr probe
DE60323068T DE60323068D1 (en) 2002-03-15 2003-03-13 The flow-through cryogenic NMR PROBE

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US36455902P 2002-03-15 2002-03-15
US60/364,559 2002-03-15

Publications (3)

Publication Number Publication Date
WO2003079034A2 WO2003079034A2 (en) 2003-09-25
WO2003079034A3 WO2003079034A3 (en) 2003-12-18
WO2003079034B1 true WO2003079034B1 (en) 2004-04-01

Family

ID=28041936

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/IB2003/002430 WO2003079034A2 (en) 2002-03-15 2003-03-13 Flow-through cryogenic nmr probe

Country Status (5)

Country Link
US (1) US6838880B2 (en)
EP (1) EP1488247B1 (en)
AT (1) ATE405849T1 (en)
DE (1) DE60323068D1 (en)
WO (1) WO2003079034A2 (en)

Families Citing this family (27)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2823308B1 (en) * 2001-04-05 2003-12-19 Inst Francais Du Petrole THERMOSTATED CONTAINMENT CELL FOR SAMPLE INTENDED FOR NMR MEASUREMENTS AND A METHOD FOR ITS IMPLEMENTATION
EP1510852B1 (en) * 2002-05-28 2008-11-19 Hoya Corporation Double-sided progressive power lens
US7381207B2 (en) * 2003-06-25 2008-06-03 Endocare, Inc. Quick disconnect assembly having a finger lock assembly
US6972568B2 (en) * 2003-09-09 2005-12-06 Varian, Inc. Radially-compact NMR flow cell assemblies and methods
US7246939B1 (en) * 2003-10-23 2007-07-24 Gultekin David H Measurement of thermal diffusivity, thermal conductivity, specific heat, specific absorption rate, thermal power, heat transfer coefficient, heat of reaction and membrane permeability by nuclear magnetic resonance
EP1735631A2 (en) * 2004-04-01 2006-12-27 Liposcience, Inc. Nmr clinical analyzers and related methods, systems, modules and computer program products for clinical evaluation of biosamples
US7145340B2 (en) * 2004-11-04 2006-12-05 Broker Biospin Corporation NMR spectrometer with flowthrough sample container
JP4291304B2 (en) * 2005-07-11 2009-07-08 株式会社日立製作所 NMR probe
US7309987B2 (en) * 2005-10-28 2007-12-18 Varian, Inc. Anticipative temperature regulation of cryogenic NMR probes
US8626925B2 (en) 2005-12-16 2014-01-07 Panasonic Corporation Systems and methods for providing a selective multicast proxy on a computer network
DE102005060447B4 (en) * 2005-12-17 2012-01-05 Bruker Biospin Mri Gmbh NMR probe head with heated housing
US7378848B2 (en) * 2006-05-05 2008-05-27 M2M Imaging Corp. Magnetic resonance coil system
JP4851261B2 (en) * 2006-08-17 2012-01-11 株式会社神戸製鋼所 Cooled NMR probe head
DE102006046888B4 (en) * 2006-10-04 2010-12-16 Bruker Biospin Ag Cooled magnetic resonance probe head with a vacuum container and associated NMR measuring apparatus
US7909227B2 (en) * 2006-12-19 2011-03-22 Endocare, Inc. Cryosurgical probe with vacuum insulation tube assembly
US7719239B2 (en) * 2007-03-27 2010-05-18 Honeywell International Inc. Fast field discharge for generator over-voltage control
US7436182B1 (en) * 2007-09-21 2008-10-14 Varian, Inc. Cryogenic NMR probe capacitors with dielectric heat sinks
US7772842B2 (en) * 2008-09-17 2010-08-10 Time Medical Holdings Company Limited Dedicated superconductor MRI imaging system
CA2683411C (en) * 2009-08-31 2017-07-18 University Of New Brunswick Magnetic resonance imaging apparatus and method
JP5508081B2 (en) 2010-03-25 2014-05-28 株式会社神戸製鋼所 Flow-through NMR analyzer
JP2011203107A (en) * 2010-03-25 2011-10-13 Kobe Steel Ltd Nmr analysis device for clinical examination
EP2407796B1 (en) * 2010-07-12 2013-03-06 Bruker BioSpin Corporation NMR flow cell
FR2986609B1 (en) * 2012-02-07 2017-06-02 Commissariat Energie Atomique THERMAL INSULATION DEVICE AND METHOD FOR OPERATING SUCH A DEVICE
JP5942700B2 (en) * 2012-08-23 2016-06-29 国立大学法人京都大学 Magnetic resonance signal detection probe
GB2506851B (en) * 2012-09-28 2014-11-12 Schlumberger Holdings NMR sample containment
US9678185B2 (en) 2013-03-15 2017-06-13 Pepsico, Inc. Method and apparatus for measuring physico-chemical properties using a nuclear magnetic resonance spectrometer
CN110031785B (en) * 2019-04-29 2021-04-06 江苏麦格迈医学科技有限公司 Temperature-variable portable probe for nuclear magnetic resonance detection

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4013111C2 (en) * 1990-04-25 1994-05-26 Spectrospin Ag RF receiver coil arrangement for NMR spectrometers
DE4101473C2 (en) 1991-01-19 1994-03-24 Bruker Analytische Messtechnik Probe head for flow-through NMR spectroscopy
GB9324596D0 (en) * 1993-11-30 1994-01-19 Oxford Analytical Instr Ltd Variable temperature nmr probe
US5508613A (en) * 1994-08-29 1996-04-16 Conductus, Inc. Apparatus for cooling NMR coils
DE59508628D1 (en) * 1995-03-25 2000-09-14 Bruker Ag Faellanden RF receiver coil arrangement for NMR spectrometers
US5867026A (en) 1996-04-04 1999-02-02 Varian Associates, Inc. Flow tube for NMR probe
US6194900B1 (en) * 1998-06-19 2001-02-27 Agilent Technologies, Inc. Integrated miniaturized device for processing and NMR detection of liquid phase samples
DE10006324C1 (en) * 2000-02-12 2001-08-16 Bruker Ag Faellanden Cooled NMR probe head with device for centering the measurement sample
US20030000911A1 (en) 2001-06-27 2003-01-02 Paul Kelley Hot-fillable multi-sided blow-molded container

Also Published As

Publication number Publication date
EP1488247A2 (en) 2004-12-22
ATE405849T1 (en) 2008-09-15
DE60323068D1 (en) 2008-10-02
WO2003079034A2 (en) 2003-09-25
US6838880B2 (en) 2005-01-04
WO2003079034A3 (en) 2003-12-18
US20040004478A1 (en) 2004-01-08
EP1488247B1 (en) 2008-08-20

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