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US4940942A Expired / Lapsed US ⏱️ 0.0 years remaining

Method and apparatus for conducting variable-temperature solid state magnetic resonance spectroscopy

Assignee: Varian Inc
•
Filing: 1989-04-14
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Granted: 1990-07-10
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Expires: 2009-04-14
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Abstract

Abstract A technique and design for variable-temperature magnetic resonance spectroscopy. Designs utilizing a separate gas for control of sample temperature confine temperature gradients away from the sample. Annular seals isolate a sample gas chamber along a rotor and avoid gas mixing and other sample temperature effects. Improved resolution by avoiding temperature gradients and independence of rotational speed from sample temperature is provided.

Inventors

  • 👤 Victor J. Bartuska
  • 👤 David H. Lewis

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-30 23:30
CPC Classifications
G; G01; G01R; G01R33/00; G01R33/20; G01R33/28; G01R33/30; G01R33/31

Claims Analysis

Total Claims: 47
Claim 1
Independent Claim 90 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy comprising the steps of: a. placing a solid state sample in a rotor; b. positioning said rotor within a magnetic field; c. spinning said rotor through operation of at least one spinning gas; d. creating a temperature gradient among the gases surrounding said rotor to impact the temperature of said solid state sample; e. affirmatively confining said temperature gradient to areas of the rotor away from said solid state sample; and f. reading the magnetic resonant emissions of said sample.
Claim 2
Independent Claim 90 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy comprising the steps of: a. placing a solid state sample in a rotor; b. positioning said rotor within a magnetic field; c. spinning said rotor through operation of at least one spinning gas; d. creating a temperature gradient among the gases surrounding said rotor to impact the temperature of said solid state sample; e. affirmatively confining said temperature gradient to areas of the rotor away from said solid state sample; and f. reading the magnetic resonant emissions of said sample.
Claim 3
Dependent Claim 34 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claim 1 and further comprising the step of controlling the temperature of said solid state sample independently of said spinning gas.
Claim 4
Dependent Claim 27 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claim 2 wherein said spinning gas comprises a drive gas and a bearing gas.
Claim 5
Dependent Claim 36 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claim 3 wherein said step of controlling the temperature of said solid state sample comprises subjecting said sample to a separate sample gas.
Claim 6
Dependent Claim 44 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claim 4 wherein said step of confining the temperature gradient compromises the step of insulating the area of the rotor containing said solid state sample from other areas of the rotor.
Claim 7
Dependent Claim 44 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claim 5 wherein said step of insulating comprises the step of substantially blocking the ability of any spinning gas to mix with the sample gas in the vicinity of said rotor.
Claim 8
Dependent Claim 33 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claim 6 wherein said blocking step comprises positioning an annular stator seal around said rotor and in close proximity thereto.
Claim 9
Dependent Claim 42 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claim 4 wherein said step of insulating the rotor comprises the steps of exhausting said spinning gas away from the area of the rotor containing the solid state sample.
Claim 10
Dependent Claim 52 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claim 7 wherein said step of insulating the rotor further comprises the steps of: a. exhausting said spinning gas away from the area of the rotor containing the solid state sample; and b. providing an insulator in the rotor.
Claim 11
Dependent Claim 60 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claim 8 wherein said spinning gas comprises a drive gas and a bearing gas and wherein said step of insulating further comprises the step of establishing the pressure of said sample gas to be greater than the pressure of the spinning gas adjacent to said sample gas.
Claim 12
Dependent Claim 25 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claim 10 wherein said bearing gas is adjacent to said sample gas.
Claim 13
Dependent Claim 25 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claim 10 wherein said drive gas is adjacent to said sample gas.
Claim 14
Independent Claim 103 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy comprising the steps of: a. placing a solid state sample in a rotor; b. positioning said rotor within a magnetic field within a probe having a removable end; c. spinning said rotor through operation of at least one spinning gas; d. creating a temperature gradient among the gases surrounding said rotor to impact the temperature of said solid state sample through operation of a sample gas; e. separating the direction from which said spinning gas and said sample gas are supplied to the rotor; f. reading the magnetic resonant emissions of said sample.
Claim 15
Independent Claim 103 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy comprising the steps of: a. placing a solid state sample in a rotor; b. positioning said rotor within a magnetic field within a probe having a removable end; c. spinning said rotor through operation of at least one spinning gas; d. creating a temperature gradient among the gases surrounding said rotor to impact the temperature of said solid state sample through operation of a sample gas; e. separating the direction from which said spinning gas and said sample gas are supplied to the rotor; f. reading the magnetic resonant emissions of said sample.
Claim 16
Dependent Claim 28 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claim 13 wherein said spinning gas is supplied through said removable end of the probe.
Claim 17
Independent Claim 41 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claims 4, 7, or 11 and further comprising the step of separating the direction from which said spinning gas and said sample gas are supplied to the rotor.
Claim 18
Dependent Claim 40 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claim 15 wherein rotor is positioned within a probe having a removable end and wherein said spinning gas is supplied through the removable end of said probe.
Claim 19
Independent Claim 51 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claims 1, 4, 7, or 11 wherein each of said gases supplied are exhausted away from said stator and further comprising the step of combining said exhaust gases into an exhaust tube in the vicinity of said stator.
Claim 20
Dependent Claim 26 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claim 17 wherein said exhaust tube has a relatively large cross sectional area.
Claim 21
Dependent Claim 61 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claim 18 wherein said sample gas is supplied through a sample gas supply line having a cross sectional area and wherein said cross sectional area of the exhaust tube is at least as large as the sum of the cross sectional areas of all the gas supply lines.
Claim 22
Dependent Claim 47 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claim 13 wherein each of said gases supplied are exhausted away from said stator and further comprising the step of combining said exhaust gases into an exhaust tube in the vicinity of said stator.
Claim 23
Dependent Claim 26 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claim 20 wherein said exhaust tube has a relatively large cross sectional area.
Claim 24
Dependent Claim 60 words
A method of performing variable-temperature, solid state magnetic resonance spectroscopy as described in claim 21 wherein said sample gas is supplied through sample gas supply line having a cross sectional area and wherein said cross sectional area of the exhaust tube is at least as large as the sum of the cross sectional areas of all the gas supply lines.
Claim 25
Dependent Claim 83 words
A variable-temperature sample spinning mechanism for conducting solid state magnetic resonance spectroscopy comprising: a. a rotor designed to contain a solid state sample; b. a stator housing surrounding said rotor and to be contained within a magnetic field; c. a means for spinning said rotor, said spinning means supplying at least one spin gas against said rotor; and d. a means for controlling the temperature of said solid state sample wherein said controlling means is independent of said means for spinning the rotor.
Claim 26
Dependent Claim 83 words
A variable-temperature sample spinning mechanism for conducting solid state magnetic resonance spectroscopy comprising: a. a rotor designed to contain a solid state sample; b. a stator housing surrounding said rotor and to be contained within a magnetic field; c. a means for spinning said rotor, said spinning means supplying at least one spin gas against said rotor; and d. a means for controlling the temperature of said solid state sample wherein said controlling means is independent of said means for spinning the rotor.
Claim 27
Dependent Claim 29 words
A variable-temperature sample spinning mechanism for conducting solid state magnetic resonance spectroscopy as described in claim 23 wherein said spin gas comprises a drive gas and a bearing gas.
Claim 28
Dependent Claim 33 words
A variable-temperature sample spinning mechanism for conducting solid state magnetic resonance spectroscopy as described in claim 24 wherein said means for controlling comprises a sample gas which is separate from said spinning gases.
Claim 29
Dependent Claim 31 words
A variable-temperature sample spinning mechanism for conducting solid state magnetic resonance spectroscopy as described in claim 25 and further comprising a means for insulating said sample gas from said spinning gases.
Claim 30
Dependent Claim 34 words
A variable-temperature sample spinning mechanism for conducting solid state magnetic resonance spectroscopy as described in claim 26 wherein said insulation means comprises an annular stator seal around said rotor and in close proximity thereto.
Claim 31
Dependent Claim 38 words
A variable-temperature sample spinning mechanism for conducting solid state magnetic resonance spectroscopy as described in claim 26 wherein said insulation means comprises at least one duct positioned to draw the spinning gases away from said solid state sample.
Claim 32
Dependent Claim 40 words
A variable-temperature sample spinning mechanism for conducting solid state magnetic resonance spectroscopy as described in claim 26 wherein said insulation means comprises at least one pressure valve for adjusting the relative pressures of said sample gas and said spinning gases.
Claim 33
Dependent Claim 72 words
A variable-temperature sample spinning mechanism for conducting solid state magnetic resonance spectroscopy as described in claim 26 wherein said insulation means comprises: a. an annular stator seal around said rotor and in close proximity thereto; b. at least one duct positioned to draw the spinning gases away from said solid state sample; and c. at least one pressure valve for adjusting the relative pressures of said sample gas and said spinning gases.
Claim 34
Dependent Claim 45 words
A variable-temperature sample spinning mechanism for conducting solid state magnetic resonance spectroscopy as described in claim 29 wherein a spinning gas is adjacent to said sample gas and wherein the pressure of said adjacent spinning gas is less than the pressure of said sample gas.
Claim 35
Dependent Claim 26 words
A variable-temperature sample spinning mechanism for conducting solid state magnetic resonance spectroscopy as described in claim 31 wherein said adjacent spinning gas is the bearing gas.
Claim 36
Dependent Claim 30 words
A variable-temperature sample spinning mechanism for conducting solid state magnetic resonance spectroscopy as described in claim 31 wherein said spinning gas adjacent to said sample gas is the drive gas.
Claim 37
Dependent Claim 125 words
A variable-temperature sample assembly for conducting solid state magnetic resonance spectroscopy comprising: a. a rotor designed to contain a solid state sample; b. a stator housing surrounding said rotor and contained within a magnetic field and within a probe having a removable end; c. a means for spinning said rotor, said spinning means supplying at least one spin gas next to said rotor through utilization of at least one spin gas supply line; d. a means for controlling the temperature of said solid state sample, said controlling means supplying a sample gas in the vicinity of said solid state sample through a sample gas supply line; and wherein said sample gas supply line and said spin gas supply line approach the rotor from opposite directions.
Claim 38
Dependent Claim 125 words
A variable-temperature sample assembly for conducting solid state magnetic resonance spectroscopy comprising: a. a rotor designed to contain a solid state sample; b. a stator housing surrounding said rotor and contained within a magnetic field and within a probe having a removable end; c. a means for spinning said rotor, said spinning means supplying at least one spin gas next to said rotor through utilization of at least one spin gas supply line; d. a means for controlling the temperature of said solid state sample, said controlling means supplying a sample gas in the vicinity of said solid state sample through a sample gas supply line; and wherein said sample gas supply line and said spin gas supply line approach the rotor from opposite directions.
Claim 39
Dependent Claim 31 words
A variable-temperature sample assembly for conducting solid state magnetic resonance spectroscopy as described in claim 34 wherein said spin gas supply line is fed through said removable end of the probe.
Claim 40
Dependent Claim 39 words
A variable-temperature sample spinning mechanism for conducting solid state magnetic resonance spectroscopy as described in claims 25, 27, or 32 wherein said sample gas and said spinning gas are supplied in the vicinity of the rotor from opposite directions.
Claim 41
Dependent Claim 43 words
A variable-temperature sample spinning mechanism for conducting solid state magnetic resonance spectroscopy as described in claim 36 wherein said rotor is positioned within a probe having a removable end and wherein said spinning gas is fed through said removable end of the probe.
Claim 42
Dependent Claim 44 words
A variable-temperature sample spinning mechanism for conducting solid state magnetic resonance spectroscopy as described in claims 23, 25, 27, or 32 and further comprising an exhaust junction connected so to combine at least two exhaust gases and so as to feed an exhaust tube.
Claim 43
Dependent Claim 28 words
A variable-temperature sample spinning mechanism for conducting solid state magnetic resonance spectroscopy as described in claim 38 wherein said exhaust tube has a relatively large cross sectional area.
Claim 44
Dependent Claim 62 words
A variable-temperature sample spinning mechanism for conducting solid state magnetic resonance spectroscopy as described in claim 39 wherein all of said gases are supplied through gas supply lines, each having a cross sectional area, and wherein said cross sectional area of the exhaust tube is at least as large as the sum of all the cross sectional areas of said supply lines.
Claim 45
Dependent Claim 39 words
A variable-temperature sample assembly for conducting solid state magnetic resonance spectroscopy as described in claim 34 and further comprising an exhaust junction connected so to combine at least two exhaust gases and so as to feed an exhaust tube.
Claim 46
Dependent Claim 27 words
A variable-temperature sample assembly for conducting solid state magnetic resonance spectroscopy as described in claim 41 wherein said exhaust tube has a relatively large cross sectional area.
Claim 47
Dependent Claim 61 words
A variable-temperature sample assembly for conducting solid state magnetic resonance spectroscopy as described in claim 42 wherein all of said gases are supplied through gas supply lines, each having a cross sectional area, and wherein said cross sectional area of the exhaust tube is at least as large as the sum of all the cross sectional areas of said supply lines.

References Cited (Backward Citations)

US4301410A Cited
US4306878A Cited
US4510450A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1993-07-09 1994-01-08 1994-07-10 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1997-07-09 1998-01-08 1998-07-10 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2001-07-09 2002-01-08 2002-07-10 $7700.00 Window Closed / Lapsed

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