Portable analytical system for detecting organic chemicals in water

• US 8,302,458 B2
• Filed: 04/21/2008
• Issued: 11/06/2012
• Est. Priority Date: 04/20/2007
• Status: Active Grant

• Current Assignee: Parker Intangibles LLC (Parker-Hannifin Corporation)
• Original Assignee: Parker-Hannifin Corporation
• Inventors: Cost, William M., Mowry, Curtis D., Siegal, Michael P., Robinson, Alex, Whiting, Joshua J., Howell, Stephen W., Ali Hassan, Kazi Zulfiqur
• Primary Examiner(s): LARKIN, DANIEL SEAN
• Application Number:
  US12/106,734
• Publication Number:
  US 20080289397A1
• Time in Patent Office: 1,660 Days
• Field of Search: 73/234, 73/240.1, 73/240.6
• US Class Current: 73/23.4
• CPC Class Codes: G01G 23/3728 with wireless means
• CPC Class Codes: G01G 3/16 measuring variations of frequency of oscillations of the body
• CPC Class Codes: G01N 2030/0095 Separation specially adapted for use outside laboratory, e.g. field sampling, portable equipments
• CPC Class Codes: G01N 2291/014 Resonance or resonant frequency
• CPC Class Codes: G01N 2291/0256 Adsorption, desorption, surface mass change, e.g. on biosensors
• CPC Class Codes: G01N 2291/0423 Surface waves, e.g. Rayleigh waves, Love waves
• CPC Class Codes: G01N 29/022 Fluid sensors based on microsensors, e.g. quartz crystal-microbalance [QCM], surface acoustic wave [SAW] devices, tuning forks, cantilevers, flexural plate wave [FPW] devices microdevices per se B81B
• CPC Class Codes: G01N 29/2462 Probes with waveguides, e.g. SAW devices
• CPC Class Codes: G01N 30/76 Acoustical detectors measurement of mechanical vibrations or ultrasonic, sonic or infrasonic waves G01H

Abstract

A portable analytical system for detecting organic chemicals in water comprising a miniature preconcentrator and a SAW detector, the latter being characterized by a nanoporous carbon coating that provides improved response compared to prior art polymer coatings, particularly when detecting low concentrations of trihalomethane chemicals, such as chloroform and bromoform.

Claims

1. A portable field system for detecting trihalo-methane compounds in water comprising:

a preconcentrator for collecting the trihalomethane compounds found in the water, wherein the preconcentrator includes one or more metal collection tubes containing therein a dual bed including a porous polymer resin material followed by a carbon-based adsorbent resin;

a recirculation loop for circulating carrier gas exiting the preconcentrator back through the preconcentrator;

a gas chromatograph column for separating the compounds as desorbed from the preconcentrator; and

a surface acoustic wave detector for determining the mass of the compounds separated by the gas chromatograph, wherein the surface acoustic wave detector has a sensing surface with a nanoporous carbon coating.

2. A system as set forth in claim 1, wherein the surface acoustic wave detector changes its frequency depending on the mass of compound adsorbed and desorbed on the sensing surface.

3. A system as set forth in claim 1, wherein the nanoporous carbon coating was applied by pulsed laser deposition.

4. A system as set forth in claim 3, wherein the carbon coating has a carbon density of about 0.8 to about 1.3 g/cm³ and a coating thickness of about 1 to about 3 μ

m.

5. A system as set forth in claim 1, wherein the operating frequency of the surface acoustic wave detector is greater than 10 MHz and less than 200 MHz.

6. A system as set forth in claim 1, wherein the operating frequency of the surface acoustic wave detector is greater than 50 MHz and less than 150 MHz.

7. A system as set forth in claim 1, wherein the operating frequency of the surface acoustic wave detector is about 100 MHz.

8. A system as set forth in claim 1, further comprising a data acquisition device for receiving and processing a frequency output of the surface acoustic wave detector.

9. A system as set forth in claim 1, wherein the preconcentrator includes a porous polymer resin material as an adsorber.

10. A system as set forth in claim 1, wherein the one or more metal collection tubes have a diameter less than 0.20 inch OD, and a heating wire wrapped around the tube.

11. A system as set forth in claim 10, wherein the one or more metal collection tubes have an outer diameter of about 0.042 inch, and are coated on its inner and outer diameter surfaces with a passivating material.

12. A system as set forth in claim 1, further comprising flow control devices for directing flow through the one or more collection tubes in one direction during adsorption and in the reverse direction during desorption.

13. A system as set forth in claim 1, further comprising a sample purger for purging chemicals from a sample for adsorption in the preconcentrator.

14. A system as set forth in claim 1, wherein the one or more collection tubes are disposed between upstream and downstream manifold blocks.

15. A system as set forth in claim 1, further comprising a supply of helium for use as a carrier gas.

16. A portable field instrument for detecting purgeable trihalomethane compounds in water, comprising:

a sample vessel wherein chemicals are purged from the water and entrained in a carrier gas;

a preconcentrator connected to the sample purger for adsorbing the chemicals from the carrier gas, wherein the preconcentrator includes one or more metal collection tubes containing therein a dual bed including a porous polymer resin material followed by a carbon-based adsorbent resin;

a recirculation loop for circulating carrier gas exiting the preconcentrator back through the sample vessel;

a heater for heating the preconcentrator for desorbing the trihalomethane compounds;

a gas chromatograph column to which the desorbed compounds are passed from the preconcentrator;

a heater for heating the gas chromatograph column for causing the compounds to desorb after different retention times in the gas chromatograph column; and

a surface acoustic wave detector to which the compounds are sequentially passed from the gas chromatograph column, the frequency of the surface acoustic wave detector changing as a function of the mass of compound adsorbed and desorbed from a sensing surface of the surface acoustic wave detector, whereby the mass quantity of the compounds is measured by the change of frequency of the surface acoustic wave device, wherein the surface acoustic wave detector has a sensing surface with a nanoporous carbon coating.

17. An instrument as set forth in claim 16, comprising a carrier gas supply for supplying to the sample vessel, air from the atmosphere as a carrier gas.

18. An instrument as set forth in claim 17, wherein the instrument has a sensitivity on the order of parts per billion or less.

19. A method for detecting in the field organic trihalomethane compounds in water comprising:

bringing a portable field instrument to a testing site;

using a preconcentrator in the instrument to collect the trihalomethane compounds from in the water, wherein the preconcentrator includes one or more metal collection tubes containing therein a dual bed including a porous polymer resin material followed by a carbon-based adsorbent resin;

using a recirculation loop in the instrument to circulate carrier gas exiting the preconcentrator back through the preconcentrator;

using a gas chromatograph column in the instrument to separate the compounds as desorbed from the preconcentrator; and

using a surface acoustic wave detector in the instrument to determine the mass of the compounds separated by the gas chromatograph, wherein the surface acoustic wave detector has a sensing surface with a nanoporous carbon coating.