IP Library Granted Patent US 8,181,544
Granted Patent B2
US 8,181,544 · App. 12/313,375 · Granted May 22, 2012

Liquid sample evaporator for vapor analysis

Assignees: Picarro, Inc.; The Regents of the University of Colorado
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Quick Facts
Patent No.
US 8,181,544
App. No.
12/313,375
Granted
May 22, 2012
Kind
B2
Abstract

Preparation methods for introducing liquid samples to gas analysis instruments include 1) complete evaporation of a liquid sample in a sample chamber, and 2) allowing the sample vapor in the sample chamber to equilibrate for a predetermined time. An inert carrier gas (e.g., dry nitrogen or zero air) is also admitted to the sample chamber. After equilibration, the sample vapor is admitted as a conditioned sample to an analysis instrument. Preferably, the predetermined equilibration time is sufficiently long that the sample vapor in the sample chamber becomes substantially homogeneous with respect to both concentration and isotopic ratio. Vapor derived from a liquid calibration standard in this manner can be employed as an accurate gas-phase calibration reference.

Claims (38)

1. A method of preparing a liquid sample for analysis, the method comprising:

admitting a first liquid sample to a sample chamber;

completely evaporating said first liquid sample in said sample chamber to provide sample vapor;

admitting a carrier gas to said sample chamber;

allowing said sample vapor and said carrier gas to statically equilibrate for a predetermined time to provide a conditioned sample in said sample chamber;

providing said conditioned sample as an output for analysis.

2. The method of claim 1 , wherein said predetermined time is selected such that said conditioned sample has substantially uniform sample vapor concentration within said sample chamber.

3. The method of claim 1 , wherein said predetermined time is selected such that said conditioned sample has substantially uniform sample vapor isotopic ratio within said sample chamber.

4. The method of claim 1 , wherein said first liquid sample is a calibration standard, and further comprising using said conditioned sample as a calibration reference for said analysis.

5. The method of claim 4 , further comprising performing alternating measurements of said calibration reference and a gaseous sample, whereby measurements of said gaseous sample calibrated with respect to said first liquid sample are provided.

6. The method of claim 4 , further comprising performing alternating measurements of said calibration reference and a second liquid sample, whereby measurements of said second liquid sample calibrated with respect to said first liquid sample are provided.

7. The method of claim 1 , wherein said analysis comprises isotopic ratio analysis.

8. The method of claim 1 , wherein said analysis includes determination of sample vapor concentration.

9. The method of claim 1 , wherein said analysis includes determination of one or more analyte concentrations in said first liquid sample.

10. The method of claim 1 , wherein said first liquid sample comprises water.

11. The method of claim 1 , further comprising performing one or more dry flush steps prior to said admitting a first liquid sample to said sample chamber, wherein each of said dry flush steps comprises:

admitting a dry carrier gas substantially free of vapor of said first liquid sample to said sample chamber, followed by

removing said dry carrier gas from said sample chamber.

12. The method of claim 1 , further comprising performing one or more wet flush steps prior to said admitting a first liquid sample to said sample chamber, .wherein each of said wet flush steps comprises:

admitting a wet carrier gas including vapor of said first liquid sample to said sample chamber, followed by

removing said wet carrier gas from said sample chamber.

13. The method of claim 1 , further comprising substantially evacuating said sample chamber prior to said admitting said first liquid sample.

14. The method of claim 13 , wherein said substantially evacuating said sample chamber is performed prior to admitting said carrier gas.

15. The method of claim 1 , further comprising maintaining said chamber at an elevated temperature.

16. The method of claim 1 , wherein all of said carrier gas is admitted to said sample chamber before said first liquid sample is admitted to said sample chamber.

17. The method of claim 1 , wherein all of said carrier gas is admitted to said sample chamber after said first liquid sample is admitted to said sample chamber.

18. The method of claim 1 , wherein some of said carrier gas is admitted to said sample chamber before said first liquid sample is admitted to said sample chamber, and wherein some of said carrier gas is admitted to said sample chamber after said first liquid sample is admitted to said sample chamber.

19. The method of claim 1 , further comprising determining a calibration of system memory.

20. The method of claim 19 , further comprising providing corrected analysis output results based on said calibration of system memory and a predetermined model of system memory effects.

21. The method of claim 20 , wherein said predetermined model is a two-term linear combination of a current measurement and a measurement immediately prior to said current measurement.

22. The method of claim 20 , wherein said predetermined model is a linear combination of a current measurement and one or more measurements prior to said current measurement.

23. The method of claim 1 , wherein said first liquid sample is. admitted to said sample chamber using a septum and syringe.

24. The method of claim 1 , wherein said first liquid sample is admitted to said sample chamber using a syringe pump or metering pump.

25. The method of claim 1 , wherein a volume of said first liquid sample is between 0.1 microliters and 10 microliters.

26. A method of preparing a liquid sample for analysis, the method comprising:

repeating the method of claim 1 two or more times, each repetition having a corresponding sample volume of said first liquid sample;

wherein an average sample volume is defined to be an average of said sample volumes;

wherein said sample volumes differ from said average sample volume by less than 10% of said average sample volume.

Assignments (5)
RELEASE OF SECURITY INTEREST Recorded Jun 2, 2021
From: SILICON VALLEY BANK
To: PICARRO, INC.
Reel/Frame 057252/0674 →
SECURITY AGREEMENT Recorded Feb 28, 2012
From: PICARRO, INC.
To: SILICON VALLEY BANK
Reel/Frame 027771/0576 →
CONFIRMATORY LICENSE Recorded Sep 28, 2009
From: PICARRO, INC
To: NATIONAL INSTITUTES OF HEALTH (NIH), U.S. DEPT. OF HEALTH AND HUMAN SERVICES (DHHS), U.S. GOVERNMENT
Reel/Frame 023288/0401 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 26, 2009
From: VAUGHN, BRUCE H.; WHITE, JAMES W. C.
To: THE REGENTS OF THE UNIVERSITY OF COLORADO
Reel/Frame 022344/0520 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 26, 2009
From: CROSSON, ERIC; RICHMAN, BRUCE A.
To: PICARRO, INC.
Reel/Frame 022344/0833 →
Continuity (1)
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