Method and apparatus for preconcentration for analysis purposes of trace constitutes in gases

• US 5,142,143 A
• Filed: 10/30/1991
• Issued: 08/25/1992
• Est. Priority Date: 10/31/1990
• Status: Expired due to Term

• Current Assignee: ABB Process Analytics, Inc. (ABB Limited)
• Original Assignee: Extrel Corporation
• Inventors: Penn, Stephen M., Fite, Wade L.
• Primary Examiner(s): Berman, Jack I.
• Assistant Examiner(s): NGUYEN, KIET TUAN
• Application Number:
  US07/784,068
• Time in Patent Office: 300 Days
• Field of Search: 250/288, 250/288 A, 250/281, 250/282, 73/863.12, 73/864.81, 73/31.01, 73/31.02, 73/31.03, 436/161, 436/173, 436/178, 422/83, 422/89
• US Class Current: 250/288
• CPC Class Codes: G01M 3/202 using mass spectrometer detection systems
• CPC Class Codes: G01N 1/405 by adsorption or absorption
• CPC Class Codes: G01N 33/0049 for halogenated organic compounds
• CPC Class Codes: Y10T 436/24 Nuclear magnetic resonance, electron spin resonance or other spin effects or mass spectrometry
• CPC Class Codes: Y10T 436/255 including use of a solid sorbent, semipermeable membrane, or liquid extraction

Abstract

A preconcentrator for analyzing trace constituents in gases wherein a sample gas is introduced to a confined sorbent which thereafter is evacuated by a vacuum pump and a low-pressure carrier gas passes through the sorbent while it is desorbing, wherein the desorbed trace constituents are carried by the carrier gas to a detector that operates at low pressure such as a mass spectrometer. Because the mass of the carrier gas which carries the desorbed trace consituents to the detector is at a lower pressure and therefore has less density than the sample gas, the relative mass of trace constituents in the carrier gas is much greater than in the sample gas. The sample gas can be hot to assist desorption or a gas which reacts with trace constituents of interest to improve their detection. Valves located in the system between the sample gas intake, the carrier gas supply, the vacuum pump for the system and the detector operate to admit the sample gas, isolate the system, create a vacuum in the system, establish the sample gas flow, and to carry the trace consituents to the detector. Preconcentrators can be placed in parallel, whereby when one is desorbing and analyzing trace elements, the other is receiving the sample gas.

Claims

1. A method of preconcentrating trace constituents in a gas for subsequent analysis which comprises the steps of:

A adsorbing at least one of the trace constituents onto a confined sorbent material for a predetermined period of time from a sample gas moving at a predetermined gaseous mass flow rate;

B confining said sorbent material in a sealed space which includes an inlet of a detector means for receiving said one trace constituent; and

C desorbing said one trace element from said sorbent material for a predetermined period of time into a carrier gas moving at a predetermined gaseous mass flow rate which is substantially less than the gaseous mass flow rate of said sample gas whereby the desorbed amount of said one trace constituent relative to said carrier gas that contains said desorbed trace constituent is substantially greater than the same amount of said one trace constituent relative to the portion of said sample gas that contained said trace constituent.

2. A method in accordance with claim 1, wherein said carrier gas containing said one trace constituent is introduced into said detector means through said inlet.

3. A method in accordance with claim 2, wherein said detector means comprises a mass spectrometer.

4. A method in accordance with claim 1, wherein the pressure of said carrier gas is substantially less than the pressure of said sample gas.

5. A method in accordance with claim 4, wherein said sample gas is substantially at or near ambient atmospheric pressure.

6. A method in accordance with claim 1, wherein said sample gas is air.

7. A method in accordance with claim 1, wherein said sorbent material is composed of particles of a solid material which are confined within a glass tube.

8. A method in accordance with claim 1, wherein said one trace constituent is caused to desorb from said sorbent material by heating said sorbent material.

9. A method in accordance with claim 8, wherein said carrier gas is preheated to assist in the desorption of said one trace constituent from said sorbent material.

10. A method in accordance with claim 1, wherein said carrier gas is air.

11. A method in accordance with claim 1, wherein said carrier gas does not chemically react with said one trace constituent.

12. A method in accordance with claim 1, wherein said carrier gas chemically reacts with said one trace constituent to produce a derivative of said one trace constituent that facilitates its detection by said detector means.

13. A method in accordance with claim 1, wherein a plurality of confined sorbent materials are provided in parallel with sealing means for each whereby one or more of said plurality of adsorbent materials may be used selectively to receive said sample gas and to desorb said carrier gas for analysis by said detector means.

14. A method in accordance with claim 3, wherein said mass spectrometer includes an electron-impact ionization ion source operatively connected to said inlet.

15. A method in accordance with claim 3, wherein said mass spectrometer includes a chemical ionization ion source operatively connected to said inlet.

16. A method in accordance with claim 15, wherein said carrier gas is a reagent gas for chemical ionization.

17. A method in accordance with claim 3, wherein said mass spectrometer includes a gas discharge ion source operatively connected to said inlet to operate at a pressure less than atmospheric pressure.

18. A method in accordance with claim 17, wherein a portion of said carrier gas entering said gas discharge ion source is removed therefrom by a vacuum pump and the remainder of said carrier gas is drawn through an aperture into the high vacuum of said mass spectrometer.

19. An apparatus for preconcentrating trace constituents in a gas to facilitate their analysis which comprises:

a sorbent material which is retained in a confined space and associated with means for selectively causing said sorbent material to adsorb or desorb said trace constituents;

a sample gas source and valve for introducing said sample gas onto said sorbent material and means for selectively opening and closing said valve;

a source of carrier gas connected to provide said carrier gas to said sorbent material;

pumping means for selectively lowering the pressure in said confined space containing said sorbent material;

a detector for detecting said trace constituents in said carrier gas;

a confined passageway from said carrier gas source to said detector through said sorbent material, whereby when said sorbent material desorbs said trace constituents received from said sample gas they can be carried by said carrier gas to said detector at a pressure substantially less than the pressure of said sample gas, whereby the ratio of the density of said trace constituents to mass of said carrier gas is substantially increased relative to the ratio of the density of said trace constituents for a comparable mass of said sample gas.

20. An apparatus in accordance with claim 19, wherein said detector comprises a mass spectrometer.

21. An apparatus in accordance with claim 20, wherein said mass spectrometer includes an electron-impact ionization ion source.

22. An apparatus in accordance with claim 20, wherein said mass spectrometer includes a chemical ionization ion source.

23. An apparatus in accordance with claim 22, wherein said carrier gas is a reagent gas to react with said trace constituents.

24. An apparatus in accordance with claim 20, wherein said mass spectrometer includes a gas discharge ion source that operates at a pressure less than atmospheric pressure.

25. An apparatus in accordance with claim 24, wherein a portion of said carrier gas entering said gas discharge ion source is removed therefrom by a vacuum pump and the remainder is removed through an aperture leading to a high vacuum in said mass spectrometer.