Parts per trillion detector

• US 6,319,723 B1
• Filed: 11/12/1998
• Issued: 11/20/2001
• Est. Priority Date: 11/12/1998
• Status: Expired due to Fees

• Current Assignee: Edward M. Ejzak, Eldon L. Jeffers
• Original Assignee: Edward M. Ejzak, Eldon L. Jeffers
• Inventors: Ejzak, Edward M., Jeffers, Eldon L.
• Primary Examiner(s): SNAY, JEFFREY R
• Application Number:
  US09/191,091
• Time in Patent Office: 1,104 Days
• Field of Search: 422/82.02, 422/88, 422/90, 436/133, 436/146, 436/177, 436/178
• US Class Current: 436/133
• CPC Class Codes: B01D 1/305 Demister (vapour-liquid separation)
• CPC Class Codes: B01D 3/00 Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping evaporation in general, e.g. of liquids for gas phase reactions B01B1/005; gas chromatography B01D15/08; destructive distillation C10B; preparation of alcoholic beverages by distillation C12H6/02
• CPC Class Codes: B01D 53/30 Controlling by gas-analysis apparatus regulating non electrical variables in general G05D
• CPC Class Codes: G01N 1/40 Concentrating samples
• CPC Class Codes: G01N 2001/4033 sample concentrated on a cold spot, e.g. condensation or distillation
• CPC Class Codes: G01N 33/0016 by regulating a physical variable, e.g. pressure or temperature
• CPC Class Codes: G01N 33/0019 by preconcentration
• CPC Class Codes: Y10T 436/204998 Inorganic carbon compounds
• CPC Class Codes: Y10T 436/235 In an aqueous solution [e.g., TOC, etc.]
• CPC Class Codes: Y10T 436/255 including use of a solid sorbent, semipermeable membrane, or liquid extraction

Abstract

An apparatus is disclosed which is capable of detecting a selected gas in a liquid sample to a sensitivity in the range of 10 to 10,000 parts per trillion. Such sensitivity is achieved by concentrating the selected gas in a sample without concentrating sources of ionic interference that are also present in the sample. Selective concentration of the gas is achieved by vaporizing the sample, correcting for non-ideal vaporization, selectively condensing the selected gas from the vapor, and detecting the selected gas. Methods for using the apparatus and detecting the selected gas are also disclosed.

Claims

1. An apparatus for detecting a selected gas in a liquid sample, the apparatus comprising;

a concentrator to concentrate the selected gas in the sample without concentrating sources of ionic interference, comprising;

a vaporizer to expel the selected gas out of the liquid sample and to evaporate at least a portion of the liquid sample to form vapor;

a mist trap in fluid communication with the vaporizer to capture mist droplets from the vaporizer; and

,

a condenser in fluid communication with the mist trap to condense the vapor to a liquid condensate, whereby the selected gas in the vapor is sorbed and concentrated in the liquid condensate; and

,

a detector in fluid communication with the concentrator to detect the selected gas in the sample.

2. The apparatus of claim 1, wherein the concentrator is tilted from the horizontal.

3. The apparatus of claim 1, further comprising a reactor in fluid communication with the concentrator to react the sample prior to concentration.

4. The apparatus of claim 1, where in the apparatus is adapted for continuous process monitoring applications.

5. The apparatus of claim 1, wherein the apparatus operates in batch mode.

6. The apparatus of claim 1, wherein the apparatus is adapted for total carbon/total inorganic carbon analysis of a sample.

7. The apparatus of claim 1, further comprising a hydrophobic membrane attached to the concentrator to remove unabsorbed gases from the apparatus.

8. The apparatus of claim 1, wherein the detector comprises concentric tubular electrodes.

9. The apparatus of claim 1, wherein the detector detects changes in conductivity in the presence of the selected gas.

10. The apparatus of claim 1, wherein the selected gas comprises carbon dioxide.

11. The apparatus of claim 1, wherein the liquid comprises water.

12. The apparatus of claim 1, wherein the concentrator comprises inert material where the sample comes into contact with the concentrator.

13. The apparatus of claim 12, wherein the inert material comprises borosilicate glass.

14. The apparatus of claim 1, wherein the mist trap comprises inert beads.

15. The apparatus of claim 14, wherein the beads comprise borosilicate glass.

16. The apparatus of claim 1, wherein the concentrator comprises a u-tube to separate the analytical sample from a blank.

17. The apparatus of claim 1, wherein the selected gas is detected in amounts as small as 10 parts per trillion.

18. A method for detecting a selected gas in a liquid sample, the method comprising:

providing a concentrator to concentrate the selected gas in the sample without concentrating sources of ionic interference;

the concentrator comprising;

a vaporizer to expel the selected gas out of the liquid sample and to evaporate at least a portion of the liquid sample to form vapor;

a mist trap in fluid communication with the vaporizer to capture mist droplets from the vaporizer; and

,

a condenser in fluid communication with the mist trap to condense the vapor to a liquid condensate, whereby the selected gas in the vapor is sorbed and concentrated in the liquid condensate;

providing a detector in fluid communication with the concentrator to detect the selected gas in the sample;

introducing the sample into the concentrator;

concentrating the selected gas without concentrating sources of ionic interference; and

detecting the concentrated selected gas.

19. The method claim 18, further comprising reacting the sample to produce the selected gas prior to concentrating the gas.

20. The method of claim 18, wherein the method is adapted for continuous process monitoring applications.

21. The method of claim 18, wherein the method is adapted for batch mode analysis.

22. The method of claim 18, wherein the method is adapted for total carbon/total inorganic carbon analysis of a sample.

23. The method of claim 18, wherein the method is reagentless.

24. The method of claim 18, wherein the selected gas is detected in amounts as small as 10 parts per trillion.

25. A method for high sensitivity detection of CO2 in liquid water, the method comprising:

heating the liquid water to release CO2 from the heated liquid water;

evaporating at least a portion of the heated liquid water to form a vapor;

condensing the vapor to form a liquid condensate, whereby CO2 is absorbed and concentrated in the liquid condensate; and

detecting the amount of CO2 in the liquid condensate.

26. The method of claim 25, further comprising a removing any unabsorbed gases after the unabsorbed gases are released from the liquid water.

27. The method of claim 25, further comprising:

detecting the amount of CO2 in the liquid water after the CO2 has been released from the liquid water by heat to provide a baseline blank measurements.

28. The method of claim 25, wherein the method is reagentless.

29. The method of claim 25, wherein the CO2 is detected in amounts as small as 10 parts per trillion.