Method and apparatus for characterizing materials by using a mechanical resonator

• US 6,393,895 B1
• Filed: 08/12/1998
• Issued: 05/28/2002
• Est. Priority Date: 10/08/1997
• Status: Expired due to Fees

• Current Assignee: Freeslate Inc. (Unchained Labs Inc.)
• Original Assignee: Symyx Technologies Incorporated (Dassault Systemes SA)
• Inventors: Bennett, James, Matsiev, Leonid, McFarland, Eric
• Primary Examiner(s): Larkin, Daniel S.
• Assistant Examiner(s): MILLER, ROSE MARY
• Application Number:
  US09/133,171
• Time in Patent Office: 1,385 Days
• Field of Search: 73/24.01,24.03,24.04,24.05,24.06,30.01,30.04,31.01,31.02,31.03,31.05,31.06 310/360,316,320 422/68.1,75,98
• US Class Current: 73/24.06
• CPC Class Codes: B01J 2219/00704 integrated with the reactor apparatus
• CPC Class Codes: G01H 13/00 Measuring resonant frequency
• CPC Class Codes: G01N 11/16 by measuring damping effect upon oscillatory body
• CPC Class Codes: G01N 2009/006 vibrating tube, tuning fork
• CPC Class Codes: G01N 2291/014 Resonance or resonant frequency
• CPC Class Codes: G01N 2291/0224 Mixtures of three or more liquids
• CPC Class Codes: G01N 2291/0255 (Bio)chemical reactions, e.g. on biosensors
• CPC Class Codes: G01N 2291/02818 Density, viscosity
• CPC Class Codes: G01N 2291/02863 Electric or magnetic parameters
• 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 2291/0427 Flexural waves, plate waves, e.g. Lamb waves, tuning fork, cantilever
• 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 29/348 with frequency characteristics, e.g. single frequency signals, chirp signals measuring frequency of mechanical vibrations or acoustic waves in general G01H1/06, G01H3/04; measuring frequency or analysing frequency spectra G01R23/00
• CPC Class Codes: G01N 29/42 by frequency filtering or by tuning to resonant frequency
• CPC Class Codes: G01N 29/4418 with a model, e.g. best-fit, regression analysis
• CPC Class Codes: G01N 5/04 by removing a component, e.g. by evaporation, and weighing the remainder
• CPC Class Codes: G01N 9/002 using variation of the resonant frequency of an element vibrating in contact with the material submitted to analysis G01N9/34 takes precedence

Abstract

A method and apparatus for measuring properties of a liquid composition includes a mechanical resonator, such as a thickness shear mode resonator or a tuning fork resonator, connected to a measurement circuit. The measurement circuit provides a variable frequency input signal to the tuning fork, causing the mechanical resonator to oscillate. To test the properties of a liquid composition, the mechanical resonator is placed inside a sample well containing a small amount of the liquid. The input signal is then sent to the mechanical resonator and swept over a selected frequency range, preferably less than 1 MHz to prevent the liquid being tested from exhibiting gel-like characteristics and causing false readings. The mechanical resonator'"'"'s response over the frequency range depends on various characteristics of the liquid being tested, such as the temperature, viscosity, and other physical properties. Particular mechanical resonators, such as tuning fork resonators, can also be used to measure a liquid composition'"'"'s electrical properties, such as the dielectric constant and conductivity, because the tuning fork'"'"'s structure allows a high degree of electrical coupling between the tuning fork and the surrounding liquid. The mechanical resonator can be covered with a coating to impart additional special detection properties to the resonator, and multiple resonators can be attached together as a single sensor to obtain multiple frequency responses. The invention is particularly suitable for combinatorial chemistry applications, which require rapid analysis of chemical properties for screening.

Claims

1. A method for measuring a property of a plurality of liquid compositions using a plurality of tuning fork resonators, the method comprising:

providing an array of sample wells;

placing each of said plurality of liquid compositions in a separate sample well;

placing one of said plurality of tuning fork resonators in a first of said plurality of liquid compositions such that at least a portion of said one of said plurality of tuning fork resonators is surrounded by said first of said plurality of liquid compositions;

placing another of said plurality of tuning fork resonators in a second of said plurality of liquid compositions such that at least a portion of said another of said plurality of tuning fork resonators is surrounded by said second of said plurality of liquid compositions;

applying a variable frequency input signal to a measurement circuit coupled with said one of said plurality of tuning fork resonators to oscillate said one of said plurality of tuning fork resonators;

applying a variable frequency input signal to a measurement circuit coupled with said another of said plurality of tuning fork resonators to oscillate said another of said plurality of tuning fork resonators wherein the measurement circuit coupled to said one of said plurality of tuning fork resonators and the measurement circuit coupled to said another of said plurality of tuning fork resonators may be the same circuit or two separate circuits;

varying a frequency of the variable frequency input signal associated with said one of said plurality of tuning fork resonators over a predetermined frequency range to obtain a frequency-dependent resonator response of said one of said plurality of tuning fork resonators;

varying a frequency of the variable frequency input signal associated with said another of said plurality of tuning fork resonators over a predetermined frequency range to obtain a frequency-dependent resonator response of said another of said plurality of tuning fork resonators; and

analyzing the resonator responses of said one of said plurality of tuning fork resonators and said another of said plurality of tuning fork resonators to measure said property of said first of said plurality of liquid compositions and said second of said plurality of liquid compositions.

2. The method of claim 1, wherein said method measures a physical property of each liquid composition in the array of sample wells.

3. The method of claim 1, wherein the physical property measured by said method is selected from the group consisting of specific weight, temperature and viscosity.

4. The method of claim 1, wherein said method measures an electrical property of each liquid composition in the array of sample wells.

5. The method of claim 4, wherein the electrical property measured by said method is selected from the group consisting of dielectric constant and conductivity.

6. The method of claim 1, wherein said method measures an electrical property and a physical property of each liquid composition in the array of sample wells simultaneously.

7. The method of claim 6, wherein the electrical properties and physical properties measured by said method are selected from the group consisting of specific weight, viscosity, temperature, dielectric constant and conductivity.

8. The method of claim 7, wherein said method simultaneously measures at least two properties selected from the group consisting of specific weight, viscosity, temperature, dielectric constant and conductivity of each liquid composition in the array of sample wells.

9. The method of claim 1, further comprising the step of coating at least one of said plurality of tuning fork resonators with a material that modifies the characteristics of said at least one tuning fork resonators.

10. The method of claim 9, wherein the material used in said coating step is a functionality designed to change the resonator response of said at least one tuning fork resonator of a selected substance is present in the liquid composition associated with said at least one tuning fork resonator.

11. The method of claim 10, wherein said functionality used in the coating step contains receptor molecules for attracting molecules of the selected substance in the liquid composition associated with said at least one tuning fork resonator.

12. An apparatus for measuring a property of a plurality of liquid compositions, comprising:

an array of tuning fork resonators;

an array of sample wells for holding said plurality of liquid compositions;

a measurement circuit coupled with said array of tuning fork resonators, said measurement circuit having a signal generator for generating a variable frequency input signal to cause said array of tuning fork resonators to oscillate; and

a receiver coupled to the measurement circuit to output a frequency response of said array of tuning fork resonators;

wherein said measurement circuit and said receiver are coupled with said array of tuning fork resonators to obtain a frequency response associated with each of said plurality of liquid compositions.

13. The apparatus of claim 12, wherein the tuning fork comprises at least two tines, each tine including a quartz crystal center portion having at least two faces and an electrode on at least one of the two faces of said quartz crystal center portion.

14. The apparatus of claim 13, wherein said quartz crystal center portion of each tine has four faces and wherein four electrodes are connected to said quartz crystal center portion such that one electrode is coupled to each face.

15. The apparatus of claim 12, further comprising a coating material on said tuning fork resonator that modifies the characteristics of the tuning fork resonator.

16. The apparatus of claim 15, wherein said coating material is a functionality designed to change the resonator response of the tuning fork resonator if a selected substance is present in the fluid composition.

17. The apparatus of claim 16, wherein said functionality contains receptor molecules for attracting molecules of the selected substance in the fluid composition to change the resonator response.

18. An apparatus for measuring a property of a fluid composition, comprising:

a plurality of tuning fork resonators, each tuning fork resonator having a different resonator response characteristic;

means for containing the fluid composition;

a measurement circuit coupled with said plurality of tuning fork resonators, said measurement circuit having a signal generator for generating a variable frequency input signal to cause at least one of said plurality of tuning fork resonators to oscillate; and

a receiver coupled to the measurement circuit to output a frequency response of said plurality of tuning fork resonators.

19. The apparatus of claim 18, wherein each tuning fork has a different functionality, each functionality designed to change the resonator response of its associated tuning fork resonator if a selected substance corresponding with the specific coating is present in the fluid composition.