Sealed magic angle spinning nuclear magnetic resonance probe and process for spectroscopy of hazardous samples

Patent metadata

Field	Value
Publication number	US-9366736-B2
Application number	US-201314106441-A
Country	US
Kind code	B2
Filing date	Dec 13, 2013
Priority date	Dec 13, 2012
Publication date	Jun 14, 2016
Grant date	Jun 14, 2016

Abstract

A magic-angle-spinning (MAS) nuclear magnetic resonance (NMR) probe is described that includes double containment enclosures configured to seal and contain hazardous samples for analysis. The probe is of a modular design that ensures containment of hazardous samples during sample analysis while preserving spin speeds for superior NMR performance and convenience of operation.

First claim

What is claimed is:

1. A sealable Magic Angle Spinning (MAS) Nuclear Magnetic Resonance (NMR) probe, comprising:
an electrically shielded probe body having an inner enclosure that defines a first containment volume and is releasably sealed by selective compressive engagement of a sealing device to a base platform, the inner enclosure configured to enclose a stator assembly that receives a rotor containing a sample therein; and
an outer enclosure that defines a second containment volume therein, and is adaptably sealable by secured connection to the probe body the outer enclosure when secured to the probe body covers the inner enclosure preventing release of the sample materials in the event of a breach in the inner enclosure or release of the sample materials within the MAS NMR probe.

2. The probe of claim 1 , wherein the inner enclosure further comprises a first gas conduit configured to deliver a high-pressure bearing gas into the inner enclosure and a second conduit configured to deliver a high-pressure spin gas through the base platform into the inner enclosure to allow for operation of the stator assembly therein when the inner enclosure is sealed.

3. The probe of claim 2 , wherein the first and second gas delivery conduits are coupled to one or more in-line check valves configured to prevent release of sample particulates.

4. The probe of claim 1 , wherein the inner enclosure includes at least one exhaust gas conduit configured to release high-pressure exhaust gas from the stator assembly through the base platform in the upper module with a capacity that preserves the spin speed of the stator assembly during operation without releasing containment when the inner enclosure is sealed.

5. The probe of claim 4 , wherein the at least one exhaust gas conduit is coupled to at least one particulate filter that is configured to remove sample particulates from the exhaust gas in the event of a release of sample particulates from the inner enclosure.

6. The probe of claim 1 , wherein the outer enclosure includes a removable containment cap comprised of a transparent polycarbonate.

7. The probe of claim 1 , wherein the inner enclosure is comprised of a transparent polycarbonate so as to allow viewing of the stator assembly within the first containment volume defined by the inner enclosure.

8. The probe of claim 1 , further comprising at least one tuning circuit electrically coupled to the stator assembly to provide tuning of resonant frequencies during operation of the probe.

9. A method for performing MAS NMR analysis, comprising:
introducing a rotor containing a sample into an electrically shielded probe body having an inner enclosure that defines a first containment volume and is adaptably sealable by secured connection to a base platform; the inner enclosure configured to enclose a stator assembly that receives the rotor containing the sample therein, the electrically shielded probe body also having an outer enclosure that defines a second volume therein, and is adaptably sealable by secured connection to the probe body;
sealing the inner enclosure containing the stator assembly by securing the inner enclosure to the base platform disposed beneath the inner enclosure to form a first containment volume within the inner enclosure;
sealing the outer enclosure by securing the outer enclosure to the probe body to form a secondary containment volume within the outer enclosure to prevent release of sample particulates in the event of a breach in the rotor or the inner enclosure within the probe during operation; and
spinning the rotor in the stator assembly.

10. The method of claim 9 , further including pre-spinning the rotor in a Contamination Area or other controlled environment located exterior to the probe to ensure the rotor containing the sample is properly sealed prior to introducing the sample into the MAS NMR probe for analysis therein.

11. The method of claim 9 , wherein the sealing step includes mounting a collar over a flange disposed at the base end of the inner enclosure and threading the collar onto inner threads that circumvolve the base platform to compress a flexible sealing component that seals the inner enclosure and the primary containment volume therein that isolates the sample within the inner enclosure of the MAS NMR probe.

12. A Magic Angle Spinning (MAS) Nuclear Magnetic Resonance (NMR) probe for containment and isolation of a sample material during analysis, the probe comprising:
a modular probe body that includes a lower module and an upper module, the upper module comprised of an outer compartment and an inner compartment each defining sample containment volumes,
the inner compartment defined by a polished polycarbonate housing that secures to a base of the probe body with a sealing collar that provides a gas-tight seal between the module and a base within the inner compartment of the probe body, whereby the base is separable from the rest of the probe body without breaching containment of the sample material from the inner compartment or the outer compartment;
the upper module further comprising:
a stator assembly coupled operatively to at least one gas inlet configured to introduce high pressure gases to the stator assembly in the inner compartment for rotation of the sample therein and at least one gas outlet to exhaust gasses from the inner compartment during operation of the NMR probe without breaching containment of material within the inner compartment.

13. The probe of claim 12 , further comprising an antenna is electrically coupled to coaxial cables, capacitors, and inductors that define an RF electrical circuit that is tuned to selected frequencies during the NMR measurement.

14. The probe of claim 12 , wherein the stator includes a fiber optic detector disposed to measure and regulate rotational speed of the MAS rotor during analysis of the sample material.

15. The probe of claim 12 , wherein the lower module further includes gas delivery conduits that are coupled to one or more in-line particulate filters that retain sample particles therein in the event of gas backflow from the inner compartment during analysis of the sample material.

Assignees

• Cho Herman M
• Washton Nancy M
• Mueller Karl T
• Sears Jr Jesse A
• Townsend Mark R
• Ewing R James
• Battelle Memorial Institute

Inventors

• Cho Herman M
• Washton Nancy M
• Mueller Karl T
• Sears Jr Jesse A
• Townsend Mark R
• Ewing R James

Classifications

• G01N24/08

  by using nuclear magnetic resonance (G01N24/12 takes precedence) · CPC title

• G01R33/465

  applied to biological material, e.g. in vitro testing · CPC title

• G01N24/084

  Detection of potentially hazardous samples, e.g. toxic samples, explosives, drugs, firearms, weapons · CPC title

• G01R33/30

  Sample handling arrangements, e.g. sample cells, spinning mechanisms · CPC title

• G01R33/307 Primary

  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 · CPC title