Infrared attenuation measuring system

• US 5,343,044 A
• Filed: 06/11/1993
• Issued: 08/30/1994
• Est. Priority Date: 09/27/1991
• Status: Expired due to Term

• Current Assignee: Foss Electric A/S
• Original Assignee: A/S Foss Electric
• Inventors: Sjaunja, Lars-Ove, Andersen, Steen K., Brems, Niels, Lapp, Torben, Nygaard, Lars, Arnvidarson, Borkur
• Primary Examiner(s): Dzierzynski, Paul M.
• Assistant Examiner(s): NOT, DEFINED
• Application Number:
  US08/075,016
• Time in Patent Office: 445 Days
• Field of Search: 250/343, 250/339, 250/340, 250/341
• US Class Current: 250/339.09
• CPC Class Codes: G01N 2021/3595 using FTIR
• CPC Class Codes: G01N 21/3577 for analysing liquids, e.g. polluted water
• CPC Class Codes: G01N 33/04 Dairy products
• CPC Class Codes: G01N 33/06 Determining fat content, e.g. by butyrometer
• CPC Class Codes: Y10S 250/91 Food sample analysis using invisible radiant energy source

Abstract

An infrared attenuation measuring system, for the quantitative determination of the concentration of one or more components in an aqueous fat-containing sample, such as milk, by an infrared attenuation technique. The system comprising a set of waveband-related parameters containing information enabling the system to calculate the concentrations substantially independent of the degree of homogenization of the fat-containing sample, and/or to determine the degree of homogenization of the sample. The parameter set contains parameters which are related to wavebands containing a high degree of information about the homogenization degree of the sample. This may be wavebands containing little information about the chemical components of the sample, and/or wavebands containing a substantial amount of information about the chemical components of the sample. The system is calibrated with aqueous fat-containing samples with different degrees of homogenization. The calculating means may be a microprocessor calculating the concentration of the component or components in question, or a neural network defined by the wave band-related parameters. The wavebands in which the attenuation values are determined in the infrared attenuation measuring means may be defined by optical filters, stationary grating and movable and/or multiple detectors, or by movable grating and one or several stationary or movable detectors. The infrared attenuation measuring means may comprise an interferometer, the data obtained from the interferometer being processed using Fourier transformation; and infrared attenuation measuring means of this type may be a FTIR spectrophotometer.

Claims

1. A method for the quantitative determination of the concentration of one or more components in an aqueous fat-containing sample by an infrared attenuation measuring technique, the method comprising measuring the infrared attenuation of a sample in one or more wavebands and calculating the concentrations of the components of the fat-containing sample from the measured infrared attenuation values of the sample using a set of waveband-related parameters, the parameter set containing information ensuring that the calculated concentrations are substantially independent of the degree of homogenization of the fat-containing sample, said information being derived from a calibration with aqueous fat-containing samples having different degrees of homogenization.

2. A method according to claim 1, wherein the parameter set has been established by a calibration performed by measuring, at different wavebands including, at least, for each component to be measured, a waveband at which the component in question influences the infrared attenuation, and a waveband at which the attenuation has a relatively high dependency on the degree of homogenization, and a relatively low dependency on the concentration of the individual components, attenuation on eithera set of samples each of which, for each component to be measured, contains a known concentration of the component, at least two of the samples containing fat of different degrees of homogenization, orat least two samples containing the same concentration of fat, but of different degrees of homogenization, a calibration having, in advance, been performed with respect to the chemical components to be measured.

3. A method according to claim 1, in which the parameter set contains parameters which are related to wavebands containing a high degree of information about the homogenization degree of the sample.

4. A method according to claim 3, wherein the wavebands containing a high degree of information about the homogenization degree of the sample comprise wavebands containing little information about the chemical components of the sample, and/or wavebands containing a substantial amount of information about the chemical components of the sample.

5. A method according to claim 1, in which the parameter set contains a parameter related to wavebands above 3400 cm^-1.

6. A method according to claim 5, wherein the parameter related to wavebands above 3400 cm^-1 is a parameter related to a waveband in the range between 3400 cm^-1 and 4000 cm^-1.

7. A method according to claim 1, in which the parameter set contains a parameter related to wavebands in the range of 2600-3400 cm^-1.

8. A method according to claim 7, in which the parameter set contains a parameter related to wavebands in the range of 2700-3100 cm^-1.

9. A method according to claim 1, in which the parameter set contains a parameter related to wavebands in the range of 2000-2600 cm^-1.

10. A method according to claim 1, in which the parameter set contains a parameter related to wavebands in the range of 800-2000 cm^-1.

11. A method according to claim 10, in which the parameter set contains a parameter related to wavebands in the range of 900-1700 cm^-1.

12. A method according to claim 10, in which the parameter set contains a parameter related to wavebands in the range of 1000-1600 cm^-1.

13. A method according to claim 10, in which the parameter set contains a parameter related to wavebands in the range of 1600-1800 cm^-1.

14. A method according to claim 1, wherein the concentrations are calculated using a linear combination of attenuation values and/or functions of attenuation values, the parameters being coefficients in the linear combination.

15. A method according to claim 1, wherein the accuracy is such that a comparison of the measured fat content of an unhomogenized raw milk sample containing 2-4% of fat with the measured fat content of a sample of the same raw milk homogenized to a mean fat globule diameter of volume of 1 μ

m, shows a relative deviation of at the most 4%.

16. A method according to claim 1, wherein the accuracy is such that a comparison of the measured fat content of an unhomogenized raw milk sample containing 2-4% of fat with the measured fat content of a sample of the same raw milk homogenized at a mean fat globule diameter of volume of 1 μ

m, shows a relative deviation of at the most 3%.

17. A method according to claim 1, wherein the accuracy is such that a comparison of the measured fat content of an unhomogenized raw milk sample containing 2-4% of fat with the measured fat content of a sample of the same raw milk homogenized at a mean fat globule diameter of volume of 1 μ

m, shows a relative deviation of at the most 2%.

18. A method according to claim 1, wherein the sample to be measured is a milk sample, and the components to be determined are selected from the group consisting of fat, protein, carbohydrates, citric acid, urea, free fatty acids, antibiotics, somatic cells, and casein.

19. A method according to claim 18, wherein the component to be determined is lactose.

20. A method according to claim 1, wherein no homogenization of the sample is performed.

35. A method according to claim 1, wherein the parameter set contains a parameter related to wavebands in the range of 2600-3400 cm^-1.

36. A method according to claim 35, wherein the parameter set contains a parameter related to wavebands in the range of 2700-3100 cm^-1.

21. A method for the quantitative determination of the concentration of one or more components in an aqueous fat-containing sample by an infrared attenuation measuring technique, the method comprising measuring the infrared attenuation of a sample in one or more wavebands and calculating the concentrations of the components of the fat-containing sample from the measured infrared attenuation values of the sample using a set of waveband-related parameters, the parameter set containing information ensuring that the calculated concentrations are substantially independent of the degree of homogenization of the fat-containing sample, so that a comparison between the measured fat content of an unhomogenized raw milk sample containing 2-4% of fat with the measured fat content of a sample of the same raw milk homogenized to a mean fat globule diameter of volume of 1 μ

m, shows a relative deviation of at the most 4%.

22. A method according to claim 21, wherein the relative deviation is at the most 3%.

23. A method according to claim 21, wherein the relative deviation is at the most 2%.

24. A method for the quantitative determination of the concentration of one or more components in an aqueous fat-containing sample by an infrared attenuation measuring technique, the method comprising measuring the infrared attenuation of a sample in one or more wavebands and calculating the concentrations of the components of the fat-containing sample from the measured infrared attenuation values of the sample using a set of waveband-related parameters, the parameters containing information being derived from a calibration with aqueous fat-containing samples having different degrees of homogenization.

25. A method for the calibration of an infrared attenuation measuring system for the quantitative determination of the concentration of one or more components in an aqueous fat-containing sample by an infrared attenuation measuring technique, the system calculating the concentrations of the components of the fat-containing sample from measured infrared attenuation values of the sample using a set of waveband-related parameters, the method comprising establishing the parameter set by calibrating the system with aqueous fat-containing samples with different degrees of homogenization.

26. A method according to claim 25, wherein the calibration is performed by measuring, at different wavebands including, at least, for each component to be measured, a waveband at which the component in question influences the infrared attenuation, and a waveband at which the attenuation has a relatively high dependency on the concentration of the individual components, attenuation on eithera set a samples each of which, for each component to be measured, contains known a known concentrations of the component, at least two of the samples containing fat of different degrees of homogenization, orat least two samples containing the same concentration of fat, but of different degrees of homogenization, the system having, in advance, being calibrated with respect to the chemical components to be measured,

and, on the basis of the resulting data sets, establishing a calibration parameter set.

27. A method according to claim 25, wherein the establishment of the set of waveband-related parameters is performed using a partial least square algorithm.

28. A method according to claim 27, wherein the establishment of the partial least square algorithm is performed using a multiple linear regression.

29. A method according to claim 25, wherein the establishment of the set of waveband-related parameters is performed using a principal component regression algorithm.

30. A method according to claim 25, wherein the number of samples corresponds to the number of wavebands, and the results of the measurements are arranged in a set of linear equations which are solved by matrix algebra to calculate the parameters.

31. A method for the determination of the degree of homogenization of an aqueous fat-containing sample by an infrared attenuation measuring technique, the method comprising measuring the infrared attenuation of the sample in one or more wavebands and calculating the degree of homogenization of the fat-containing sample from the measured infrared attenuation values of the sample using a set of waveband-related parameters containing information being derived from a calibration with aqueous fat-containing samples having different degrees of homogenization.

32. A method according to claim 31, wherein the parameter set contains parameters which are related to wavebands containing a high degree of information about the homogenization degree of the sample.

33. A method according to claim 31, wherein the parameter set contains a parameter related to wavebands above 3400 cm^-1.

34. A method according to claim 33, wherein the parameter related to wavebands above 3400 cm^-1 is a parameter related to a waveband in the range between 3400 cm^-1 and 4000 cm^-1.

37. A method according to claim 31, wherein the parameter set contains a parameter related to wavebands in the range of 2000-2600 cm^-1.

38. A method according to claim 31, wherein the parameter set contains a parameter related to wavebands in the range of 800-2000 cm^-1.

39. A method according to claim 38, wherein the parameter set contains a parameter related to wavebands in the range of 900-1700 cm^-1.

40. A method according to claim 38, wherein the parameter set contains a parameter related to wavebands in the range of 1000-1600 cm^-1.

41. A method according to claim 38, wherein the parameter set contains a parameter related to wavebands in the range of 1600-1800 cm^-1.

42. A method according to claim 31, wherein the degree of homogenization is calculated using a linear combination of attenuation values and/or functions of attenuation values, the parameters being coefficients in the linear combination.