Conformational real-time atmospheric and environmental characterization sampling apparatus and method

• US 7,288,760 B2
• Filed: 06/22/2005
• Issued: 10/30/2007
• Est. Priority Date: 06/22/2005
• Status: Active Grant

• Current Assignee: Battelle Memorial Institute
• Original Assignee: Battelle Memorial Institute
• Inventors: Weitz, Karl K.
• Primary Examiner(s): Wells; Nikita
• Assistant Examiner(s): SMITH, JOHNNIE L
• Application Number:
  US11/165,082
• Publication Number:
  US 20070023641A1
• Time in Patent Office: 860 Days
• Field of Search: 250/288, 600/532, 600/509, 356/338, 356/340
• US Class Current: 250/288
• CPC Class Codes: G01N 35/1097 characterised by the valves valves in general F16K

Abstract

The present invention relates generally to a method and apparatus for real-time environmental gas sampling. A manifold is disclosed allowing for real-time gas sampling and monitoring/analysis of atomospheric over a wide range of oxygen contents, e.g., oxygen-rich as well as oxygen-deficient sampling environments in conjunction with mass-sepectrometric analysis achieving detection limits as low as single part per-billion.

Claims

1. A method, comprising:

providing a manifold having;

a throughput valving means operable for coupling to an atmospheric sampling environment or volume;

an inlet valving means for introducing an atmospheric or other sample containing an analyte(s) of interest into a mass-selective detector, component, or instrument;

a fractioning means operably coupled to;

(i) a pumping means, (ii) said inlet valving means, and (iii) said throughput valving means for fractioning said sample; and

,

wherein said manifold is fully conformational with said sampling environment and said detector, component, or instrument whereby a selectable flow of said sample is introduced from said sampling environment or volume into said manifold by means of said throughput valving means and further into said mass-selective detector, component, or instrument at the operational vacuum or pressure for said detector, component, or instrument by means of said inlet valving means, the coordinated operation of said throughput valving means and said inlet valving means permitting sampling, monitoring, and/or analysis of said analyte(s) in said sampling environment in real-time.

2. The method of claim 1, wherein said sampling environment or volume is an oxygen-rich sampling environment or volume.

3. The method of claim 2, wherein said operational vacuum or pressure is in the range from about 0.5×

10<sup>−

5</sup> Torr to about 5×

10<sup>−

6</sup> Torr operable for monitoring and/or analysis of said analyte(s) in said oxygen-rich sampling environment or volume in real time.

4. The method of claim 1, wherein said sampling environment or volume is an oxygen-deficient sampling environment or volume.

5. The method of claim 4, wherein said operational vacuum or pressure is up to about 708 Torr operable for monitoring and/or analysis of said analyte(s) in said oxygen-deficient sampling environment in real time.

6. The method of claim 1, wherein said manifold is incorporated in a system for monitoring/analysis of a head-space(s) or volume.

7. The method of claim 1, wherein said manifold is a component of a real-time offgassing, exhausting, and/or vehicle emission monitoring or detection system.

8. The method of claim 1, wherein said manifold is a component of a system or device for real-time monitoring/detection of toxic, environmentally hazardous chemical and/or biological agents, or industrially generated analytes in a sampling environment or volume.

9. The method of claim 1, wherein said manifold is operably connected to a mass-selective detector or other mass-selective component, or is itself a component of a mass-selective instrument system.

10. A method for sampling, monitoring, and/or analysis of a gaseous atmospheric sampling environment in real time, comprising:

providing a gas transfer manifold comprising;

(i) a inlet (valving) means having a selectable flow rate for metering a sample into a mass-selective detector, component, and/or instrument;

(ii) a throughput (valving) means having a selectable flow rate operably disposed with said sampling environment or volume, whereby said sample is introduced to said manifold from said environment transferring through said manifold to said instrument, component, and/or detector;

(iii) a sample fractioning means operably disposed between said throughput (valving) means and said inlet (valving) means for fractioning of said sample in conjunction with a pumping means;

(iv) a pumping means operably disposed with said fractioning means for pulling said sample through said manifold and/or for scrubbing particulates from said sample, whereby a desired vacuum pressure to said detector, component, and/or instrument is maintained, whereby the operation of said gas manifold comprises;

determining a throughput value for sampling of said sampling environment or volume;

setting said throughput valving means at said throughput value for sampling of said sampling environment;

initiating said pumping means filling said manifold with said sample containing an analyte(s) of interest from said sampling environment and transferring said sample(s) to said mass-selective detector, component, and/or instrument;

setting said inlet valving means at a flow rate wherein the pressure of said sample introduced into said instrument, component, or mass-selective detector substantially adapting to the operational pressure or vacuum of said mass-selective detector, component, and/or instrument; and

analyzing said analyte of interest in conjunction with said mass-selective detector, component, and/or instrument, whereby said analyte from said sampling environment or volume is monitored and/or analyzed in real-time.

11. The method of claim 10, wherein said mass-selective instrument is selected from the group consisting of MS/MS, tandem MS, MSⁿ, ion-trap MS, quadrupole MS, ToF MS, FT-ICR MS, or combinations thereof.

12. The method of claim 10, wherein said inlet valving means adjusts dynamically to a pressure or vacuum in the range from about 0.5×

10<sup>−

5</sup> Torr to about 2.5×

10<sup>−

5</sup> Torr in response to the flow rate of said throughput valving means.

13. The method of claim 10, wherein said throughput valve introduces a gas sample to said manifold at a flow rate in the range from about 1 mL/min. to about 400 mL/min.

14. The method of claim 10, wherein said fractioning means comprises a member selected from the group consisting of 3-port valve, 4-port. valve, n-port valve, “

T”

connector, or combinations thereof.

15. The method of claim 10, wherein said mass-selective detector, component and/or instrument further comprises a primary ionization source or filament in a mass spectrometer instrument configuration and/or system.

16. The method of claim 15, wherein said primary ionization source is a glow discharge ionization source.

17. The method of claim 10, wherein said pumping means is selected from the group consisting of foreline pump, vacuum pump, turbo pump.

18. The method of claim 10, further comprising a selective elution system or device for concentration, desorption, and temperature dependent release of a multiplicity of analytes for monitoring/detection of a sampling environment.

19. A gas manifold, comprising:

a throughput valving means operable for coupling to an atmospheric or other sampling environment;

an inlet valving means for introducing an atmospheric or environmental sample containing an analyte(s) of interest into a mass-selective detector, component, or instrument;

a pumping means operably coupled to said inlet valving means and said throughput valving means for pulling said sample through said manifold; and

,

wherein the manifold is fully conformational with said sampling environment and said detector, component, or instrument whereby a selectable flow of said sample is introduced into said mass-selective detector, component, or instrument at the operational vacuum or pressure for said detector, component, or instrument by said inlet valving means, the coordinated operation of said throughput valving means and said inlet valving means permitting sampling, monitoring, and/or analysis of said analyte(s) in said sampling environment in real-time.

20. The manifold of claim 19, wherein said mass-selective instrument is selected from the group consisting of MS/MS, tandem MS, MSⁿ, ion-trap MS, quadrupole MS, ToF MS, FT-ICR MS, or combinations thereof.

21. The manifold of claim 19, wherein said pressure is in the range from about 0.5×

10<sup>−

5</sup> Torr to about 2.5×

10<sup>−

5</sup> Torr operable for monitoring and/or analysis of said analyte(s) in an oxygen-rich sampling environment in real time.

22. The manifold of claim 19, wherein said inlet valving means comprises a digital mass flow controlled inlet valve whereby said operational vacuum pressure of said mass-selective detector, component, and/or instrument is maintained.

23. The manifold of claim 19, wherein said pressure is up to about 608 torr operable for monitoring and/or analysis of said analyte(s) in an oxygen-deficient sampling environment in real time.

24. The manifold of claim 19, wherein said operational vacuum or pressure is measured in conjunction with an ion gauge vacuum monitor.

25. The manifold of claim 19, wherein said inlet valving and throughput valving means are selected from the group consisting of electric or pneumatic vacuum valves, pressure valves, mass-flow controller, metering valves, digital versions thereof, and combinations thereof.

26. The manifold of claim 19, further comprising a selective elution system or device for capture, desorption, concentration, and temperature dependent release of a multiplicity of analytes collected from a sampling environment permitting monitoring/detection of said analytes from said environment in real-time.

27. The manifold of claim 19, wherein said manifold is a component of a system for monitoring/analysis of a sampling environment comprising a head-space(s) or volume in real-time.

28. The manifold of claim 19, wherein said manifold is a component of a real-time offgassing, exhausting, and/or vehicle emission monitoring or detection system.

29. The manifold of claim 19, wherein said manifold is a component of a system or device for real-time monitoring/detection of toxic, environmentally hazardous chemical and/or biological agents, or industrially generated analytes in a sampling environment or volume.

30. The manifold of claim 19, wherein said manifold is a component of a mass-selective detector, mass-selective component, or mass-selective instrument system.

31. A gas manifold, comprising:

adjustable throughput valving means operable for coupling to an atmospheric sampling environment;

adjustable inlet valving means for, introducing a gas sample into a mass-selective detector, component, or instrument;

fractioning means operably coupled to;

(i) a pumping means, (ii) said inlet valving means, and (iii) said throughput valving means; and

,

wherein said throughput valving means and said inlet valving means are operably coupled providing coordinated adjustment whereby said manifold is fully conformational with both said sampling environment and said detector, component, or instrument, said manifold introducing a selectable flow of said gas sample into said mass-selective detector, component, or instrument at a operational vacuum or pressure optimized for said detector, component, and/or instrument operable for sampling, monitoring, and/or analysis of an analyte(s) from said atmospheric sampling environment in real-time.

32. The manifold of claim 31, wherein said fractioning means comprises a vacuum pump and a member selected from the group consisting of vacuum T-union, 3-way union, 4-way union, 3-way connector, T-connector, 4-way connector, or combinations thereof.

33. The manifold of claim 31 wherein said fractioning means comprises a foreline vacuum pump, said fractioning means operably linked with said inlet valve for fractionating the amount of said gas sample input to said mass-selective detector, selective detector, component, and/or instrument thereby maintaining said operational vacuum or pressure of said mass-selective detector, component, and/or instrument.

34. The manifold of claim 31, further comprising a particulate trap disposed between said pumping means and said fractioning means for trapping particulates removed from said sample permitting characterization of said particulates.

35. The manifold of claim 31, wherein said manifold is a component of a particulate analysis instrument or system.