High-sensitivity instrument to measure NVR in fluids

• US 6,363,773 B1
• Filed: 04/18/2000
• Issued: 04/02/2002
• Est. Priority Date: 07/11/1996
• Status: Expired due to Fees

• Current Assignee: Femtometrics, Inc. (BAE Systems Plc)
• Original Assignee: Femtometrics, Inc. (BAE Systems Plc)
• Inventors: Bowers, William D.
• Primary Examiner(s): Williams, Hezron
• Assistant Examiner(s): MILLER, ROSE MARY
• Application Number:
  US09/552,462
• Time in Patent Office: 714 Days
• Field of Search: 73/240.1, 73/240.6, 73/310.6, 73/32.A, 73/544.1, 735/99, 73/617.9, 310/313.D, 310/313.B, 310/313.R, 310/312
• US Class Current: 73/24.06
• CPC Class Codes: G01N 2291/0224 Mixtures of three or more liquids
• CPC Class Codes: G01N 2291/0256 Adsorption, desorption, surface mass change, e.g. on biosensors
• CPC Class Codes: G01N 2291/0422 Shear waves, transverse waves, horizontally polarised waves
• CPC Class Codes: G01N 2291/0423 Surface waves, e.g. Rayleigh waves, Love waves
• CPC Class Codes: G01N 2291/0426 Bulk waves, e.g. quartz crystal microbalance, torsional waves
• CPC Class Codes: G01N 2291/101 one transducer
• 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 29/036 by measuring frequency or resonance of acoustic waves
• CPC Class Codes: G01N 29/222 Constructional or flow details for analysing fluids optoacoustic fluid cells G01N29/2425

Abstract

A real time nonvolatile residue (NVR) monitor operates to efficiently detect molecular contamination in a given environment. The present NVR monitor utilizes surface acoustic wave (SAW) resonators in a controlled environment which efficiently promotes deposition of NVR on the sensor surface. The SAW resonators preferably operate at a resonant frequency of approximately 200 MHz-2,000 MHz which enables the NVR monitor to detect molecular contamination on the order of 10⁻¹¹ g-cm⁻² to 10⁻¹³ g-cm⁻². The NVR monitor utilizes active temperature control of (SAW) resonators to achieve a stable resonant frequency and to thermally separate NVR from a sample fluid contacting the SAW. The temperature control system of the NVR monitor is able to directly heat and cool the SAW resonators utilizing a thermoelectric element to maintain the resonators at a preset temperature in accordance with optimal environmental conditions for separating NVR from the sample fluid. The sample fluid, comprising a carrier fluid and NVR, is furthermore processed to provide conditions, such as pre-cooling and/or pressurization, which enhance condensation of NVR on the sensor surface. Increasing the collection efficiency allows the NVR monitor to operate faster at a desired level of accuracy and provides more quantitative information for trace contaminant analysis.

Claims

1. A method of detecting contaminants in an otherwise pure fluid, comprising:

transporting a mixture of said fluid and contaminants from a vessel into a fluid inlet of a detection apparatus;

transporting said mixture from said fluid inlet along a flow path to a SAW sensor of said apparatus such that the only contaminants reaching said SAW sensor originate from said vessel;

delivering said mixture of said fluid and said contaminants from said flow path to said SAW sensor such that a surface of the SAW sensor is exposed to said mixture;

controlling the temperature of the mixture as said mixture flows along the flow path;

thermally separating the contaminants from the fluid in the delivered mixture such that said contaminants are distributed on the surface of the SAW sensor; and

detecting changes in response of the SAW sensor due to the contaminants on the surface of the SAW sensor.

2. The method of claim 1, wherein the fluid comprises a liquid, and wherein the step of delivering comprises coating the surface of the SAW sensor with a uniformly thick layer of said liquid.

3. The method of claim 2, wherein the step of coating comprises spraying the liquid onto the surface of the SAW sensor.

4. The method of claim 1, wherein the step of delivering the fluid to the SAW sensor comprises flowing the fluid through a fluid dispenser disposed adjacent to the surface of the SAW sensor such that the fluid travels in a substantially linear path from the fluid dispenser to the surface of the SAW sensor.

5. The method of claim 1, wherein the fluid comprises a liquid, and wherein the step of thermally separating the contaminants from the liquid comprises maintaining the SAW sensor at a temperature sufficient to induce evaporation of the liquid from the surface of the SAW sensor while leaving contaminants thereon.

6. The method of claim 1, wherein the fluid comprises a gas, and wherein the step of thermally separating the contaminants from the gas comprises maintaining the SAW sensor at a temperature sufficient to induce condensation of the contaminants onto the surface of the SAW.

7. The method of claim 1, wherein the detecting step comprises detecting changes in frequency response of the SAW sensor by detecting a beat frequency between said SAW sensor and a reference sensor.

8. The method of claim 1, further comprising the step of identifying molecular species of the contaminants by determining a mass spectrum of the molecular species.

9. A method of detecting contaminants in an otherwise pure fluid comprising:

transporting a mixture of said fluid and contaminants from a vessel into a fluid inlet of a detection apparatus;

transporting said mixture from said fluid inlet along a flow path to a SAW sensor of said apparatus such that the only contaminants reaching said SAW sensor originate from said vessel;

delivering said mixture of said fluid and said contaminants from said flow path to said SAW sensor such that a surface of the SAW sensor is exposed to said mixture;

precooling the delivered mixture prior to delivering the mixture to the SAW sensor;

thermally separating the contaminants from the fluid in the delivered mixture such that said contaminants are distributed on the surface of the SAW sensor; and

detecting changes in response of the SAW sensor due to the contaminants on the surface of the SAW sensor.

10. The method of claim 9, wherein the step of precooling the delivered mixture comprises substantially adiabatically cooling the mixture.

11. The method of claim 9, wherein the step of precooling the delivered mixture comprises substantially isenthalpically cooling the mixture.

12. An apparatus for detecting contaminants in an otherwise pure liquid contained in a vessel, comprising:

a SAW sensor having a sensor surface;

a liquid inlet adapted for connection to said vessel so as to receive a mixture of said contaminants and said otherwise pure liquid from said vessel;

a liquid dispenser which receives the same mixture received by said inlet and dispenses said same mixture onto the SAW sensor surface such that the only contaminants dispensed onto said SAW sensor originate in said vessel;

a sample reservoir that receives said same mixture received by said inlet and supplies said same mixture to said liquid dispensers; and

a temperature controller that controls the temperature of said SAW sensor such that said contaminants are thermally separated from said liquid and distributed on the surface of the SAW sensor.

13. The method of claim 12, wherein the temperature of the mixture is controlled as said mixture flows along the flow path such that said contaminants are not deposited on any surface prior to being delivered to said SAW sensor.