Electro-optical analyzer for measuring percentage by weight of fat, protein and lactose in milk

• US 4,310,763 A
• Filed: 10/15/1979
• Issued: 01/12/1982
• Est. Priority Date: 10/15/1979
• Status: Expired due to Term

• Current Assignee: Multispec Ltd. (NWF Group PLC)
• Original Assignee: John Shields
• Inventors: Shields, John
• Primary Examiner(s): Willis, Davis L.
• Application Number:
  US06/084,662
• Time in Patent Office: 820 Days
• Field of Search: 250/339, 250/338, 250/340, 250/341, 250/343, 250/344, 250/345, 356/432, 356/433, 356/435, 356/436, 356/440, 356/441, 356/442
• US Class Current: 250/339.1
• CPC Class Codes: G01J 1/24 using electric radiation detectors
• CPC Class Codes: G01N 21/251 Colorimeters; Construction thereof
• CPC Class Codes: G01N 2201/0446 Multicell plate, sequential
• CPC Class Codes: G01N 2201/127 Calibration; base line adjustment; drift compensation
• CPC Class Codes: G01N 33/04 Dairy products
• CPC Class Codes: Y10S 250/91 Food sample analysis using invisible radiant energy source

Abstract

Electro-optical apparatus for measurement of fat, protein, lactose and water or solids in milk wherein a milk sample is pumped by a homogenizer into an optical measurement cell. The specimen in the cell is then irradiated with reference and measurement beams at differing wavelengths for fat, protein, lactose and water respectively, and signals are stored indicative of uncorrected concentrations. A scaling and correction circuit includes cross-correction circuitry for compensating the effects on each reading caused by the other constituents. The signals so corrected are then provided in percentage by weight or weight over volume on suitable digital displays.

Claims

1. Apparatus for quantitative analysis of optical characteristics of fluent materials comprising a source of radiation in the infrared spectrum, first means for splitting radiation from said source into first and second convergent beams, a drum disposed to rotate about a fixed axis and having a circumferential rim portion disposed to intersect one of said beams as said drum is rotated and an axial disc portion disposed to intersect the other of said beams as said drum is rotated, an optically transparent cell aligned with said first beam for holding a test sample, chopper means disposed between said drum and said cell and adapted to alternate between a first position in which said first beam is directed through said cell and a second position in which said second beam is directed through said cell, optical filter means disposed in said disc and rim portions of said drum as to intersect respective ones of said beams such that said chopper means alternately directs first and second beams through said cell at wavelengths corresponding to said filter means in said first and second positions of said chopper means, and energy responsive means disposed to be responsive to radiation transmitted through said cell for indicating an optical characteristic of a test sample within said cell.

2. The apparatus set forth in claim 1 wherein said rim is substantially cylindrical and said disc portion is perpendicular to said rim portion, and wherein said first and second beams are orthogonally convergent after passage through said filter means.

3. The apparatus set forth in claim 2 wherein said cell is disposed on axis with one of said first and second beams, and wherein said chopper means comprises a rotatable disc disposed at the zone of intersection of said first and second beams and having a first transparent circumferential portion for passing said first beam to said cell and a second reflective circumferential portion angulated to reflect the other of said first and second beams on axis to said cell.

4. The apparatus set forth in claim 3 wherein said filter means comprise first and second series of optical filters respectively disposed in said rim and disc portions of said drum with filters in said first and second series being grouped in coordinated pairs on radii from the radiation axis of said drum such that filters in said pairs simultaneously intersect associated ones of said first and second beams.

5. The apparatus set forth in claim 4 for quantitative analysis of a multiplicity of optical characteristics of a test sample contained in said cell, each said filter pair comprising a reference filter and a measurement filter for passing light to said cell at differing preselected wavelengths such that one of said characteristics is manifested by a difference in energy absorption at said differing wavelengths, wherein said light responsive means includes circuit means responsive to said difference in energy absorption for measuring said one characteristic.

6. The apparatus set forth in claim 5 further comprising means for step-wise rotation of said drum for locating each of said filter pairs in said beam, said circuit means being responsive to differences in energy absorption at the said differing wavelengths of each said filter pair for measuring each said characteristic, and control means coupled to said drum for controlling said circuit means as a function of the filter pair intersecting said beams.

7. The apparatus set forth in claim 6 further comprising adjustable first energy shutter means disposed to intersect one of said beams, and means coupled to said control means for adjustably positioning said first shutter means within said one beam at a position selected for each said filter pair to provide a zero indication of optical characteristics at said radiation responsive means in the absence of a sample in said cell.

8. The apparatus set forth in claim 6 wherein said filter means comprises first and second series of absorption filters each selected to transmit radiation in a band around a selected nominal peak wavelength, said first and second series being adapted to transmit wavelengths in a selected range of the infrared spectrum, and wherein said radiation source includes interference filter means for transmitting to said absorption filters substantially only energy within said range so as to minimize heating of said absorption filters.

9. The apparatus set forth in claim 6 for measuring fat, protein and lactose concentrations in milk wherein said reference and measurement filters are grouped in pairs having respective nominal peak transmission wavelengths of about 3.47μ

and 3.418μ

for fat, 6.68μ and

6.46μ

for protein, and 7.67μ and

9.6μ

for lactose.

10. The apparatus set forth in claim 9 for further measuring water concentration in milk wherein said reference and measurement filters are grouped in an additional pair possessing respective nominal peak transmission wavelengths of about 5.55μ

and 4.7μ

for measurement of water concentration.

11. In an apparatus for quantitative analysis of optical characteristics of materials comprising an infrared source, an optically transparent cell for holding a test sample, means for splitting energy from said source into first and second beams, means for alternately directing said first and second beams through said cell, energy responsive means disposed to receive radiation transmitted through said cell alternately in said first and second beams, and radiation filter means disposed to intersect said first and second beams such that radiation incident on said energy responsive means in said first and second beams exhibit differing wavelength characteristics, the improvement wherein said beam splitting means comprises means for splitting said beam into a said first beam on a first axis which intersects said cell and energy responsive means, and a said second beam on a second axis orthogonally intersecting said first axis, wherein said filter means comprises rotatable means having first and second series of filters disposed in orthogonal pairs and means for stepwise rotation of said rotatable means such that selected ones of said first and second filter series comprising said pairs are alternately positioned to intersect said first and second beams, and wherein said means for alternately directing said beams through said cell comprises a chopper having a transparent portion and a reflective portion, means positioning said chopper at the area of intersection of said first and second axes at an orientation of 45°

with respect to both said axes, and means for rotating said chopper such that, in alternation, said first beam is transmitted by said transparent portion to said cell and said second beam is reflected by said second portion to said cell.

12. The apparatus set forth in claim 11 wherein said first and second beams are substantially confocal at said cell.

13. The apparatus set forth in claim 12 wherein said beam splitting means comprise first and second plane mirrors reflecting light from said source, a first spherical mirror disposed to receive said first beam from said first plane mirror and to focus said first beam at said cell, and a second spherical mirror disposed to receive said second beam from said second plane mirror and to cooperate with said reflective position of said disc to focus said second beam at said cell, and wherein said apparatus further comprises an ellipsoidal mirror having a first focus at said cell and a second focus at said light responsive means.

14. The apparatus set forth in claim 11 wherein said energy responsive means comprises thermoelectric means disposed such that first and second beams are alternately incident thereon, shutter means adapted to be adjustably positioned in one of said first and second beams, servo means coupled to said thermoelectric means and responsive to differing intensity of said first and second beams alternately incident on said thermoelectric means for adjustably positioning said shutter means in said one of said beams until said intensities are equal, and means responsive to said servo means for indicating said optical characteristics.

15. The apparatus set forth in claim 14 wherein said servo means comprises a pivot arm carrying said shutter means, a servo motor electrically connected to said light responsive means, transmission means coupling said pivot arm to said motor, and a coil spring coupled to said pivot arm for biasing said pivot arm and said transmission means against said motor such that said motor exhibits substantially zero backlash.

16. Apparatus for spectrophotometric absorption analysis of material comprising a source of infrared radiation means including means for generating first and second divergent beams from said source, a cell for holding a test sample of material, first reflective means disposed in the path of said first beam for focusing said first beam at said cell on an optical axis, detection means, ellipsoidal reflective means having a first focus at said cell and a second focus at said detection means, second reflective means disposed in the path of said second beam for redirecting said second beam to intersect said first beam orthogonally to said axis and to focus said second beam, means disposed at the zone of intersection of said first and second beams for alternately and sequentially directing said first and second beams through said cell such that said second beam is substantially confocal with said first beam when directed through said cell, filter means having a first portion disposed to intersect said first beam between said first reflective means and said means for alternately directing said beams through said cell, a second portion orthogonal to said first portion and disposed to intersect said second beam between said second reflective means and said means for alternately directing said beams, first and second series of optical filters respectively disposed on said first and second portions in coordinated pairs such that filters in said pairs simultaneously intersect said first and second beams and means for alternately locating selected one of said filter pairs in said beams, and means coupled to said detection means and responsive to differing intensity of beams passing through each said filter pair and through said cell for measuring optical characteristics of the test sample.

17. Apparatus for optically analyzing fluid emulsions such as milk which comprises an optically transparent cell for holding a sample of said emulsion of predetermined quantity, means including a homogenizer having an inlet to receive said fluid emulsion and an outlet for providing a quantity of homogenized fluid substantially in excess of said predetermined quantity, first conduit means for directing fluid from said homogenizer through said sample cell, second conduit means operatively connected to said first conduit means upstream of said cell for routing fluid to bypass said cell, control means coupled to said homogenizer means, said first conduit means and said second conduit means for directing a first measured quantity of homogenized fluid through said first conduit means and said second conduit means bypassing said cell so as to purge said homogenizer and said first conduit means and then for directing a second measured quantity of homogenized fluid through said first conduit means to said cell, and means responsive to said control means for directing an optical beam through said cell so as to analyze fluid in said cell for a selected optical characteristic.

18. The apparatus set forth in claim 17 wherein said control means comprises a first control valve disposed in one of said first and second conduit means and operate when open to permit passage of fluid through the associated said conduit means, and means for closing said control valve for directing fluid through the other of said conduit means.

19. The apparatus set forth in claim 18 wherein said control means further comprises a second control valve disposed in the said other of said conduit means, said second control valve including means normally closing said second control valve so as to resist passage of said fluid through said other conduit means when said first control valve is open and means responsive to increase in pressure in said other conduit means when said first control valve is closed to open said second control valve.

20. The apparatus set forth in claim 19 wherein said homogenizer includes two valves and a hydraulic diaphragm pump for receiving and directing fluid emulsion through said valves, wherein said means including said homogenizer includes means for providing pulsed hydraulic energy to said diaphragm pump such that said quantity of fluid appears in pulses, and wherein said control means further comprises means coupled to said pulsed hydraulic energy providing means and to said first control valve for directing a series of first pulses through said first and second means bypassing said cell for purging said first conduit means and a series of second pulses through said first conduit means both to purge said cell and to fill said cell with filtered fluid to be analyzed.

21. The apparatus set forth in claim 20 wherein said cell comprises a pair of opposed windows separated by a space for holding test material, and wherein said first and second conduit means are of resilient tubular construction for elastically absorbing impulse fluid pressure from said homogenizer and thereby preventing flexure of said cell windows.

22. The apparatus set forth in claim 21 wherein said second series of pulses comprises one pulse of emulsion substantially in excess of that needed to fill said cell.

23. The apparatus set forth in claim 22 for analyzing milk further comprising means mounted to said homogenizer for heating said homogenizer to a temperature above room temperature.

24. The apparatus set forth in claim 23 wherein said temperature is substantially 40°

C.

25. The apparatus set forth in claim 17 further comprising filter means disposed at the junction of said first and second conduit means, such that said second measured quantity of fluid flowing through said first conduit means to said cell passes through and is filtered by said filter means, while said first measured quantity of fluid flowing through said first and second conduit means bypasses and tends to wash said filter means.

26. The apparatus set forth in claim 17 wherein said sample cell comprises a pair of flat parallel optical windows and means spacing said windows from each other to provide a generally planar sample zone, fluid inlet and outlet ports including openings extending through one of said windows and spaced from each other such that fluid entering said inlet port traverses said zone between said windows before exiting said outlet port, a fluid passage extending past said inlet port and connecting with said inlet port through an opening in a side wall of said passage, and a filter medium carried against said passage side wall across said opening such that fluid which enters said zone through said inlet port is filtered by said filter medium while fluid passing through said passage past said inlet port tends to wash said filter medium.

27. The apparatus set forth in claim 26 wherein said cell further comprises a plate having a flat surface carried in facing engagement with the other of said windows externally of said zone, passages extending through said other window and opening into said zone, and a groove in said flat plate surface in fluid communication with said passages in said other window such that a quantity of fluid entering said zone through said inlet port bypasses said zone by passing through said passages in said other window and through said groove.

28. The apparatus set forth in claim 27 wherein said plate has a central opening for passage of an optical beam through said windows, wherein said groove is generally circular surrounding said opening in said plate, and wherein said passages in said other window are substantially aligned with said openings extending through said one window.