Fluid quality control using broad spectrum impedance spectroscopy

• US 7,049,831 B2
• Filed: 02/16/2004
• Issued: 05/23/2006
• Est. Priority Date: 02/16/2004
• Status: Expired due to Fees

• Current Assignee: Eaton Corp. (Wisconsin) (Eaton Corporation PLC.)
• Original Assignee: Eaton Corp. (Wisconsin) (Eaton Corporation PLC.)
• Inventors: Hirthe, Richard Walter, Seitz, Martin Arthur, Wooton, David Lee
• Primary Examiner(s): DEB, ANJAN K
• Application Number:
  US10/778,896
• Publication Number:
  US 20050179449A1
• Time in Patent Office: 827 Days
• Field of Search: 324/698, 324/691, 324/76.22, 702/25, 702/76, 702 81- 84, 73/530.1, 73/530.5, 436/150
• US Class Current: 324/698
• CPC Class Codes: G01N 27/026 Dielectric impedance spectroscopy electrochemical impedance spectroscopy for measuring corrosion G01N17/02
• CPC Class Codes: G01N 33/2888 Lubricating oil characteristics, e.g. deterioration lubricating properties G01N33/30

Abstract

A system and method for monitoring and controlling the properties of fluids is disclosed. The inventive concept employs impedance spectroscopy (IS) measurements, and is suitable for real-time, in situ, monitoring and quality control operations, such as quality control during the manufacture of blended lubricants. IS data are obtained for three or more frequencies, where the lowest frequency is less than 1 Hz and the highest frequency is greater than 1 Hz. These data may be interpreted according to statistical techniques such as Principal Component Regression, analytical techniques such as equivalent circuit modeling, or by a combination thereof. The data analysis provides characteristics, or IS signatures, relating to the properties of the fluid. IS signatures for a test fluid are compared to IS signatures for calibration fluids to determine whether the properties of the test fluid fall within specified limits. Quality control adjustments to the test fluid properties may be performed based on the IS signatures.

Claims

1. A fluid property quality control method, comprising the steps of:

a) obtaining a set of calibration fluids representative of a manufacturing process;

b) performing impedance measurements on each of the calibration fluids to obtain first impedance spectroscopy (IS) data, wherein the first IS data include data for at least three frequencies;

c) analyzing the first IS data providing first IS signatures indicative of properties for each of the calibration fluids;

d) performing impedance measurements on a test fluid providing second IS data, wherein the second IS data include data for at least three frequencies;

e) analyzing the second IS data providing second IS signatures indicative of properties of the test fluid;

f) comparing the first IS signatures and the second IS signatures providing quality control information relating to the properties of the test fluid; and

g) modifying the manufacturing process responsive to the quality control information;

wherein the step of analyzing the first IS data and the step of analyzing the second IS data include equivalent circuit modeling, and the first IS signatures and the second IS signatures include at least one of the following;

a bulk fluid resistance R_fluid, a bulk fluid capacitance C_fluid, a bulk fluid time constant τ

_fluid, an interface capacitance C_dl, a charge transfer resistance R_ct, an interface time constant τ

_i, an interface resistance R_i, a Constant Phase Element Q_i, a Constant Phase Element exponent n, a film time constant τ

_film, a film resistance R_film, and a film capacitance C_film.

2. The fluid property quality control method of claim 1, wherein the set of calibration fluids include calibration fluids having selected concentrations of at least one additive in a base fluid, and wherein the selected concentrations are representative of desired concentration limits for the at least one additive.

3. The fluid property quality control method of claim 2, wherein the base fluid includes at least one component from the following categories:

mineral base oil and synthetic base oil.

4. The fluid property quality control method of claim 3, wherein the at least one additive includes at least one component selected from the following categories:

viscosity modifiers, pour point depressants, stabilizers, seal swell agents, anti-static additives, antioxidants, metal deactivators, anti-foam agents, detergents, dispersants, anti-wear additives, and corrosion inhibitors.

5. The fluid property quality control method of claim 1, wherein the step of analyzing the first IS data and the step of analyzing the second IS data include statistical techniques.

6. The fluid property quality control method of claim 5, wherein the statistical techniques include at least one of the following:

Principal Component Analysis, Multivariate Least Squares Regression, Principal Component Regression, Pattern Recognition analysis, Cluster analysis, Neural Net analysis, and Group Methods of Data Handling.

7. The fluid property quality control method of claim 6, wherein the first IS signatures and the second IS signatures include principal components.

8. The fluid property quality control method of claim 1 wherein the frequencies of step a) and step d) each include at least one frequency less than one Hertz, and at least one frequency greater than one Hertz.

9. The fluid property quality control method of claim 1, wherein the test fluid is a lubricant.

10. The fluid property quality control method of claim 9, wherein the step of modifying the properties of the test fluid includes modifying the concentrations of additives to the lubricant.

11. The fluid property quality control method of claim 1, wherein the test fluid is a lubricant additive package.

12. The fluid property quality control method of claim 11, wherein the step of modifying the properties of the test fluid includes modifying the concentrations of components in the lubricant additive package.

13. A quality control system controlling properties of a fluid, comprising:

a) an impedance spectroscopy (IS) probe operatively disposed in contact with the fluid;

b) an impedance spectrometer, operatively connected to the IS probe, wherein the impedance spectrometer performs impedance measurements on the fluid, and wherein the impedance spectrometer provides IS data for at least three distinct frequencies;

c) a data processing system, operatively connected to the impedance spectrometer receiving the IS data, wherein the data processing system provides first IS signatures indicative of the fluid properties, and wherein the data processing system provides quality control information responsive to a comparison of the first IS signatures to a set of second IS signatures, wherein the set of second IS signatures are indicative of properties of a set of calibration fluids; and

d) a Quality Control Operator, operatively disposed to receive the quality control information from the data processing system, and wherein the Quality Control Operator modifies the fluid properties in response to the quality control information;

wherein the data processing system employs equivalent circuit modeling to provide the first IS signatures, and the first IS signatures and the second IS signatures include at least one of the following;

a bulk fluid resistance R_fluid, a bulk fluid capacitance C_fluid, a bulk fluid time constant τ

_fluid, an interface capacitance C_dl, a charge transfer resistance R_ct, an interface time constant τ

_i, an interface resistance R_i, a Constant Phase Element Q_i, a Constant Phase Element exponent n, a film time constant τ

_film, a film resistance R_film, and a film capacitance C_film.

14. The quality control system of claim 13, wherein the IS probe includes concentric tubular electrodes.

15. The quality control system of claim 13, wherein the fluid is a lubricant.

16. The quality control system of claim 13, wherein the fluid is a lubricant additive package.

17. The quality control system of claim 13, wherein the data processing system includes a CPU and a memory.

18. The quality control system of claim 13, wherein the data processing system employs at least one of the following statistical techniques to provide the first IS signatures:

Principal Component Analysis, Multivariate Least Squares Regression, Principal Component Regression, Pattern Recognition analysis, Cluster analysis, Neural Net analysis, and Group Methods of Data Handling.

19. The quality control system of claim 18, wherein the first IS signatures and the second IS signatures include principal components.

20. The quality control system of claim 13, wherein the set of calibration fluids include calibration fluids having selected concentrations of at least one additive in a base fluid, and wherein the selected concentrations are representative of desired concentration limits for the at least one additive.

21. The quality control system of claim 20, wherein the base fluid includes at least one component from the following categories:

mineral base oil and synthetic base oil.

22. The quality control system of claim 20, wherein the at least one additive includes at least one component selected from the following categories:

viscosity modifiers, pour point depressants, stabilizers, seal swell agents, anti-static additives, antioxidants, metal deactivators, anti-foam agents, detergents, dispersants, anti-wear additives, and corrosion inhibitors.

23. The quality control system of claim 13, wherein the Quality Control Operator includes at least one of the following:

a person, an apparatus, and an automatic system.

24. The quality control system of claim 13, wherein the Quality Control Operator modifies the fluid properties by adjusting the concentrations of additives in the fluid.

25. The quality control system of claim 13, wherein the fluid is a lubricant, and the Quality Control Operator modifies the fluid properties by adjusting the concentrations of additives in the lubricant.

26. The quality control system of claim 13, wherein the fluid is lubricant additive package, and the Quality Control Operator modifies the fluid properties by adjusting the concentrations of components in the additive package.

27. The quality control system of claim 13, wherein the test fluid is a lubricant additive package, and the means for modifying the test fluid modifies the fluid properties by adjusting the concentrations of components in the additive package.

28. The quality control system of claim 13, wherein the first IS signatures and the second IS signatures include principal components.

29. A quality control system controlling properties of a fluid, comprising:

a) means for obtaining a set of calibration fluids representative of a manufacturing process;

b) means for performing impedance measurements at on each of the calibration fluids to obtain first impedance spectroscopy (IS) data, wherein the first IS data include data for at least three frequencies;

c) means for analyzing the first IS data providing first IS signatures indicative of properties for each of the calibration fluids;

d) means for performing impedance measurements on a test fluid providing second IS data, wherein the second IS data include data for at least three frequencies;

e) means for analyzing the second IS data providing second IS signatures indicative of properties of the test fluid;

f) means for comparing the first IS signatures and the second IS signatures providing quality control information relating to the properties of the test fluid; and

g) means for modifying the properties of the test fluid responsive to the quality control information;

wherein the means for analyzing the first IS data and the means for analyzing the second IS data employ equivalent circuit modeling, and the first IS signatures and the second IS signatures include at least one of the following;

a bulk fluid resistance R_fluid, a bulk fluid capacitance C_fluid, a bulk fluid time constant τ

_fluid, an interface capacitance C_dl, a charge transfer resistance R_ct, an interface time constant τ

_i, an interface resistance R_i, a Constant Phase Element Q_i, a Constant Phase Element exponent n, a film time constant τ

_film, a film resistance R_film, and a film capacitance C_film.

30. The quality control system of claim 29, wherein the means for performing impedance measurements includes an IS probe having concentric tubular electrodes.

31. The quality control system of claim 29, wherein the test fluid is a lubricant.

32. The quality control system of claim 29, wherein the test fluid is a lubricant additive package.

33. The quality control system of claim 29, wherein the means for analyzing the first IS data and the means for analyzing the second IS data are a data processing system.

34. The quality control system of claim 33, wherein the data processing system includes a CPU and a memory.

35. The quality control system of claim 29, wherein the means for analyzing the first IS data and the means for analyzing the second IS data employ at least one of the following statistical techniques:

Principal Component Analysis, Multivariate Least Squares Regression, Principal Component Regression, Pattern Recognition analysis, Cluster analysis, Neural Net analysis, and Group Methods of Data Handling.

36. The quality control system of claim 35, wherein the first IS signatures and the second IS signatures include principal components.

37. The quality control system of claim 29, wherein the set of calibration fluids include calibration fluids having selected concentrations of at least one additive in a base fluid, and wherein the selected concentrations are representative of desired concentration limits for the at least one additive.

38. The quality control system of claim 37, wherein the base fluid includes at least one component from the following categories:

mineral base oil and synthetic base oil.

39. The quality control system of claim 37, wherein the at least one additive includes at least one component selected from the following categories:

viscosity modifiers, pour point depressants, stabilizers, seal swell agents, anti-static additives, antioxidants, metal deactivators, anti-foam agents, detergents, dispersants, anti-wear additives, and corrosion inhibitors.

40. The quality control system of claim 29, wherein the means for modifying the test fluid includes at least one of the following:

a person, an apparatus, and an automatic system.

41. The quality control system of claim 29, wherein the test fluid is a lubricant, and the means for modifying the test fluid modifies the fluid properties by adjusting the concentrations of additives in the lubricant.

42. A fluid property quality control method, comprising the steps of:

a) obtaining a set of calibration fluids representative of a first product;

b) performing impedance measurements on each of the calibration fluids to obtain first impedance spectroscopy (IS) data, wherein the first IS data include data for at least three frequencies;

c) analyzing the first IS data providing first IS signatures indicative of properties for each of the calibration fluids;

d) performing impedance measurements on a test fluid providing second IS data, wherein the test fluid is representative of a second product, and wherein the second IS data include data for at least three frequencies;

e) analyzing the second IS data providing second IS signatures indicative of properties of the test fluid;

f) comparing the first IS signatures and the second IS signatures providing quality control information relating to the properties of the test fluid; and

g) selectively accepting the second product, responsive to the quality control information;

wherein the step of analyzing the first IS data and the step of analyzing the second IS data include equivalent circuit modeling, and the first IS signatures and the second IS signatures include at least one of the following;

a bulk fluid resistance R_fluid, a bulk fluid capacitance C_fluid, a bulk fluid time constant τ

_fluid, an interface capacitance C_dl, a charge transfer resistance R_ct, an interface time constant τ

_i, an interface resistance R_i, a Constant Phase Element Q_i, a Constant Phase Element exponent n, a film time constant τ

_film, a film resistance R_film, and a film capacitance C_film.

43. The fluid property quality control method of claim 42, wherein the first product is a genuine product.

44. The fluid property quality control method of claim 43, wherein the second product belongs to one of the following categories:

a genuine product and a counterfeit product.

45. The fluid property quality control method of claim 42, wherein the first product is a product of acceptable quality.

46. The fluid property quality control method of claim 45, wherein the second product belongs to one of the following categories:

a product of acceptable quality and a product of unacceptable quality.

47. The fluid property quality control method of claim 42, wherein the set of calibration fluids include calibration fluids having selected concentrations of at least one additive in a base fluid, and wherein the selected concentrations are representative of desired concentration limits for the at least one additive.

48. The fluid property quality control method of claim 47, wherein the base fluid includes at least one component from the following categories:

mineral base oil and synthetic base oil.

49. The fluid property quality control method of claim 48, wherein the at least one additive includes at least one component selected from the following categories:

viscosity modifiers, pour point depressants, stabilizers, seal swell agents, anti-static additives, antioxidants, metal deactivators, anti-foam agents, detergents, dispersants, anti-wear additives, and corrosion inhibitors.

50. The fluid property quality control method of claim 42, wherein the step of analyzing the first IS data and the step of analyzing the second IS data include statistical techniques.

51. The fluid property quality control method of claim 50, wherein the statistical techniques include at least one of the following:

Principal Component Analysis, Multivariate Least Squares Regression, Principal Component Regression, Pattern Recognition analysis, Cluster analysis, Neural Net analysis, and Group Methods of Data Handling.

52. The fluid property quality control method of claim 51, wherein the first IS signatures and the second IS signatures include principal components.

53. The fluid property quality control method of claim 42 wherein the frequencies of step a) and step d) each include at least one frequency less than one Hertz, and at least one frequency greater than one Hertz.

54. The fluid property quality control method of claim 42, wherein the test fluid is a lubricant.

55. The fluid property quality control method of claim 42, wherein the test fluid is a lubricant additive package.