Method and device for automatic spectrometric analysis of a liquid, particularly of milk

• US 4,855,601 A
• Filed: 10/27/1987
• Issued: 08/08/1989
• Est. Priority Date: 10/30/1986
• Status: Expired due to Fees

• Current Assignee: Societe Civile de Brevets JLS La Mayrie F-38770 La Motte D'Aveillans France
• Original Assignee: Societe Civile de Brevets JLS
• Inventors: Savoyet, Jean-Louis
• Primary Examiner(s): NOT, DEFINED
• Assistant Examiner(s): Rauchholz, William F.
• Application Number:
  US07/114,273
• Time in Patent Office: 651 Days
• Field of Search: 250/339, 250/359.1, 250/360.1, 250/358.1, 250/340, 250/341, 250/304, 250/453.1, 250/454.1, 250/455.1, 436/23, 436/44, 436/155, 422/66
• US Class Current: 250/339.12
• CPC Class Codes: G01N 33/04 Dairy products
• CPC Class Codes: G01N 35/00009 provided with a sample supporting tape, e.g. with absorbent zones
• CPC Class Codes: Y10S 250/91 Food sample analysis using invisible radiant energy source

Abstract

A method and device for automatic spectrometric analysis of a liquid, particularly of milk, is provided. A plate with an aperture is inserted into a cell containing the liquid. The plate is then withdrawn from the cell, leaving the aperture filled with a defined volume of the liquid. A jet of air is used to deposit the volume of liquid onto a plaque. The plaque is then moved into vertical alignment with the spreading device. The spreading device includes a bent wire rotatable by, for example, a motor for spreading the liquid into a circular spot. Preferably, the spot is dried while it is being spread. The plaque is then moved adjacent to a spectrometric analysis device for, for example, passing infrared radiation through the sample and to a detector, preferably configured to detect several wavelengths. The plaque carrying the sample is then moved to a cleaning station where it is cleaned by wiping the spot, preferably with a tape of filter paper wetted with detergent or solvent.

Claims

1. Method of spectrometric analysis of a liquid, by measurement of the absorption in various frequency bands of an infrared radiation, characterized in that the following operations are carried out in succession:

a small volume of the liquid to be analyzed is accurately dispensed and is deposited on the planar upper surface of a small plaque (7) of a material which is transparent to the radiation employed.

this volume of liquid is spread on the small plaque over a well-defined surface area with the aid of a rotary device,

the liquid spot thus produced is dried, until a dry spot is obtained,

the small plaque (7) carrying its dry spot is subjected to spectrometic analysis in the absence of the solvent of the liquid, and

the upper surface of the small plaque is cleaned by wiping and polishing before the next measurement.

2. A method, as claimed in claim 1, wherein said method of spectrometric analysis of a liquid comprises spectrometric analysis of milk.

3. A method, as claimed in claim 1, wherein said spreading of a volume of liquid over a well-defined surface area comprises spreading a volume of liquid over a circular surface area.

4. A method, as claimed in claim 1, wherein:

the step wherein said liquid spot is dried, is conducted at the same time as the step wherein said liquid is spread.

5. A method, as claimed in claim 1, wherein said step of automatically dispensing and depositing comprises:

providing a sliding plaque having a orifice and a non-wettable wall;

sliding said sliding plaque in a leakproof manner into a cell containing the liquid to be analyzed, wherein said orifice may be immersed in said liquid; and

sliding said sliding plaque outward through said wall of said cell to extract a cylindrical volume of liquid.

6. A method, as claimed in claim 1, wherein said depositing of a small volume comprises blowing a jet of air on said small volume to move said small volume onto said small plaque.

7. A method, as claimed in claim 1, wherein said spreading of said volume comprises:

providing a bent wire mounted at the end of a rotary spindle;

placing at least a portion of said bent wire in contact with said volume of liquid; and

rotating said rotary spindle to rotate said bent wire.

8. A method, as claimed in claim 1, wherein said cleaning of small plaque comprises:

contacting at least a portion of said small plaque with a tape; and

wiping said small plaque with said tape.

9. A method, as claimed in claim 8, further comprising wetting at least a portion of said tape with a material selected from the group consisting of detergents and solvents.

13. Device according to claim 1, characterized in that the spreading means consists of a rectangularly bent wire (26) mounted at the end of a rotary spindle (27) equipped with a means for approaching and withdrawing (29, 30, 31) for coming into contact with the small plaque (7), the whole unit being contained in an enclosure (32) fitted with a means of heating (39) and of ventilation (38).

10. A device for spectrometric analysis of a liquid comprising:

first means for dispensing of a precise volume of liquid and depositing said volume liquid on a small plaque (7),

second means for spreading of this volume over a determined surface area to allow said liquid to dry into a spot,

third means for spectrometric analysis of the small plaque (7) carrying its dry spot, and

a device for wiping with the aid of a filter-paper tape (48) with suitable detergents and solvents, a device for producing movement (8, 9,

     10), ensuring the movement of a small support-plaque (5) carrying at least one small plaque (7) to cause it to occupy the various stations in succession.

11. A device according to claim 10, characterized in that the means for dispensing the small precise volume of liquid consists of a sliding plaque (11) provided with an orifice (12) with a nonwettable wall and sliding in a leakproof manner through the wall of a cell (13) containing the liquid to be analyzed, so that the orifice may be immersed in the liquid in order to extract the precise cylindrical volume of liquid out of said cell and above the small plaque (7), this volume being purged onto this small plaque by a brief jet of air.

12. A device according to claim 11, characterized in that the said sliding plaque (11) is made of ceramic and that the orifice (12) is coated internally with a nonwetting product.

14. A device according to claim 10, characterized in that a source of infrared radiation (40) is provided which consists of a carbon filament (41) contained in a reflector (42) equipped with a Peltier cooler (43) and is closed by two discs (44, 45) separated by vacuum and made of a material which is transparent to the infrared.

15. A device according to claim 10, characterized in that a radiation detector (47) is provided made up of a network of individual detectors mounted on the same substrate and each detecting one of the frequency bands employed for the spectrometric analysis.

16. Device according to claim 10, characterized in that the frequency bands employed for the spectrometric analysis comprise at least the following three bands:

1770 to 1720 waves/cm (5.650 to 5.814 μ

m),

1580 to 1490 waves/cm (6.329 to 6.711 μ

m), and

1070 to 1000 waves/cm (9.345 to 10 μ

m).

17. A device, as claimed in claim 10, wherein said device for producing movement comprises a device for producing horizontal rectilinear movement.

18. A device according to claim 17, characterized in that the relative horizontal movement ensuring the actions of cleaning by wiping and polishing of the small plaque (7) at the cleaning station, is produced by the same device responsible for the movement of the small sample-carrier plaque (5) to the various stations, by virtue of an alternation of the two directions of travel.

19. Device according to claim 10, characterized in that the filter-paper tape (48) used for the cleaning is loaded with the aid of a cassette (51) containing both a dispensing (49) reel and a receiving (50) reel.

20. A device, as claimed in claim 10, further comprising means for drying said volume spread over a determined surface area.