Flow detectors having mechanical oscillators, and use thereof in flow characterization systems

• US 7,302,830 B2
• Filed: 06/05/2002
• Issued: 12/04/2007
• Est. Priority Date: 06/06/2001
• Status: Active Grant

• Current Assignee: Meas France
• Original Assignee: Symyx Technologies Incorporated (Dassault Systemes SA)
• Inventors: Matsiev, Leonid, Kolosov, Oleg, Petro, Miroslav
• Primary Examiner(s): Williams; Hezron
• Assistant Examiner(s): FRANK, RODNEY T
• Application Number:
  US10/163,064
• Publication Number:
  US 20030000291A1
• Time in Patent Office: 2,008 Days
• Field of Search: 73/615.2, 73/614.3, 73/614.1, 73/530.1
• US Class Current: 73/61.52
• CPC Class Codes: G01N 11/167 Sample holder oscillates, e.g. rotating crucible
• CPC Class Codes: G01N 2030/765 for measuring mechanical vibrations
• CPC Class Codes: G01N 2291/0256 Adsorption, desorption, surface mass change, e.g. on biosensors
• CPC Class Codes: G01N 2291/02818 Density, viscosity
• 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 29/4427 with stored values, e.g. threshold values
• CPC Class Codes: G01N 29/46 by spectral analysis, e.g. Fourier analysis or wavelet analysis spectral signal processing per se G06F17/14
• CPC Class Codes: G01N 30/16 Injection G01N30/24 takes precedence
• CPC Class Codes: G01N 30/76 Acoustical detectors measurement of mechanical vibrations or ultrasonic, sonic or infrasonic waves G01H
• CPC Class Codes: G01N 35/085 Flow Injection Analysis
• 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
• CPC Class Codes: G01N 9/32 by using flow properties of fluids, e.g. flow through tubes or apertures

Abstract

An improved system, device and method for characterizing a fluid sample that includes injecting a fluid sample into a mobile phase of a flow characterization system, and detecting a property of the fluid sample or of a component thereof with a flow detector comprising a mechanical resonator, preferably one that is operated at a frequency less than about 1 MHz, such as a tuning fork resonator.

Claims

1. A tuning fork resonator detector system, comprising:

an inlet conduit for receiving a fluid sample;

a head portion including a passageway for defining a detection cell in fluid communication with the inlet conduit;

a tuning fork resonator including at least one tuning fork, at least a portion of said at least one tuning fork being housed in the passageway;

an outlet conduit adapted for passage of the sample out of the head portion; and

an apparatus for performing a non-chromatographic separation of the fluid sample upstream of the head portion.

2. The detector system of claim 1, wherein the inlet conduit and the outlet conduit have cross-sectional areas smaller than a cross sectional area of the head portion.

3. The detector system of claim 1, further comprising a source of a variable frequency input signal for oscillating the tuning fork resonator.

4. A detector for a flow characterization system, comprising:

an inlet conduit for receiving a fluid sample;

a detection cell including a flow passageway in fluid communication with the inlet conduit;

a tuning fork resonator including at least one tuning fork that is operable at a frequency less than about 100 kHz, at least a portion of said at least one tuning fork being located in the flow passageway of the detection cell;

a housing associated with the detection cell and adapted for connecting the tuning fork resonator with a signal generator, a signal receiver, or a combination thereof; and

an outlet conduit in fluid communication with the flow passageway of the detection cell;

wherein the inlet conduit and the outlet conduit are disposed generally orthogonally relative to each other, and

wherein said at least one tuning fork has tines located in the detection cell in a fluid path between the inlet conduit and the outlet conduit.

5. A tuning fork resonator detector system, comprising:

a filtration apparatus for performing a non-chromatographic separation of a sample;

an inlet for receiving a liquid component of said sample downstream of the filtration apparatus;

a detection cell in fluid communication with the inlet;

a tuning fork resonator including at least one tuning fork that is operated at a frequency less than about 100 kHz, at least a portion of said at least one tuning fork being located in the detection cell; and

an outlet adapted for passage of the liquid component of said sample out of the detection cell;

wherein said at least one tuning fork has tines located in a fluid path between the inlet and the outlet; and

wherein the tuning fork resonator is adapted for measuring viscosity of the liquid component of said sample.

6. The detector system of claim 5, further comprising data acquisition hardware in signaling communication with the tuning fork resonator.

7. The detector system of claim 6, further comprising a pump for advancing the liquid component of the sample through the detection cell.

8. The detector system of claim 5, further comprising a pump for advancing the liquid component of the sample through the detection cell.

9. The detector system of claim 5, further comprising a microprocessor in electronic communication with the tuning fork resonator to collect, process and analyze data obtained therefrom.

10. The detector system of claim 7, further comprising a microprocessor in electronic communication with the tuning fork resonator to collect, process and analyze the data obtained therefrom.

11. The detector system of claim 8, wherein the microprocessor also operates the pump.

12. A tuning fork resonator detector system, comprising:

an inlet conduit for receiving a fluid sample;

a detection cell including a flow passageway in fluid communication with the inlet conduit;

a tuning fork resonator comprising at least one tuning fork having tines, at least a portion of said at least one tuning fork being located in the flow passageway of the detection cell; and

an outlet conduit in fluid communication with the flow passageway of the detection cell for discharging the sample;

the inlet conduit and the outlet conduit being disposed generally orthogonally relative to each other, and the tuning fork being orientated in the flow passageway such that bulk flow of the fluid sample is substantially parallel to primary surfaces of the tines of the tuning fork.

19. The tuning fork resonator detector system of claims 12, 14, 15 or 16 wherein the dead volume of the flow passageway of the detection cell is less than about 75 microliters.

20. The tuning fork resonator detector system of claims 12, 13, 14, 15 or 16 wherein the dead volume of the flow passageway of the detection cell is less than about 50 microliters.

21. The tuning fork resonator detector system of claims 12, 13, 14, 15 or 16 wherein the dead volume of the flow passageway of the detection cell is less than about 20 microliters.

23. The tuning fork resonator detector system of claims 12, 13, 14 or 16 wherein the detection cell has an internal volume ranging from about 1 microliter to about 500 microliters.

24. The tuning fork resonator detector system of claims 12, 13, 14, 15 or 16 wherein the detection cell has an internal volume ranging from about 5 microliters to about 50 microliters.

25. The tuning fork resonator detector system of claims 12, 13, 14 or 15 further comprising:

a library comprising a plurality of fluids, the fluids being spatially separate and addressable for sampling; and

an autosampler adapted for sampling the fluids and providing samples of the fluids to the inlet conduit.

13. A tuning fork resonator detector system, comprising:

an inlet conduit for receiving a fluid sample;

a detection cell including a flow passageway in fluid communication with the inlet conduit;

a tuning fork resonator, at least a portion of which is located in the flow passageway; and

an outlet conduit in fluid communication with the flow passageway of the detection cell for discharging the sample;

the inlet conduit and the outlet conduit being disposed relative to each other, and the tuning fork resonator being orientated in the flow passageway such that the dead volume of the flow passageway of the detection cell is less than about 75 microliters.

18. The tuning fork resonator detector system of claims 13, 14, 15 or 16 wherein the tuning fork resonator comprises at least one tuning fork having tines, the tuning fork being orientated in the flow passageway such that bulk flow of the fluid sample is substantially parallel to primary surfaces of the tines of the tuning fork resonator.

22. The tuning fork resonator detector system of claims 13, 15 or 16 wherein the inlet conduit and the outlet conduit are disposed at an obtuse angle relative to each other.

14. A tuning fork resonator detector system, comprising:

an inlet conduit for receiving a fluid sample;

a detection cell including a flow passageway in fluid communication with the inlet conduit;

a tuning fork resonator, at least a portion of which is located in the flow passageway; and

an outlet conduit in fluid communication with the flow passageway of the detection cell for discharging the sample;

the inlet conduit and the outlet conduit being disposed at an obtuse angle relative to each other.

15. A tuning fork resonator detector system, comprising:

an inlet conduit for receiving a fluid sample;

a detection cell including a flow passageway in fluid communication with the inlet conduit;

a tuning fork resonator, at least a portion of which is located in the flow passageway; and

an outlet conduit in fluid communication with the flow passageway of the detection cell for discharging the sample;

the detection cell having an internal volume ranging from about 1 microliter to about 500 microliters.

17. The tuning fork resonator detector system of claims 15 or 16 wherein the inlet conduit and the outlet conduit are disposed generally orthogonally relative to each other.

16. A tuning fork resonator detector system, comprising:

an inlet conduit for receiving a fluid sample;

a detection cell including a flow passageway in fluid communication with the inlet conduit;

a tuning fork resonator, at least a portion of which is located in the flow passageway;

an outlet conduit in fluid communication with the flow passageway of the detection cell for discharging the sample;

a library comprising a plurality of fluids, the fluids being spatially separate and addressable for sampling; and

an autosampler adapted for sampling the fluids and providing samples of the fluids to the inlet conduit.