Optical probe for remote attenuated total reflectance measurements

• US 5,436,454 A
• Filed: 10/15/1993
• Issued: 07/25/1995
• Est. Priority Date: 10/15/1993
• Status: Expired due to Term

• Current Assignee: Thermo Nicolet Corporation (Thermo Fisher Scientific Incorporated)
• Original Assignee: Nicolet Instrument Corporation (Thermo Fisher Scientific Incorporated)
• Inventors: Lowry, Stephen R., Bornstein, Aharon
• Primary Examiner(s): Hannaher, Constantine
• Assistant Examiner(s): Glick, Edward J.
• Application Number:
  US08/138,631
• Time in Patent Office: 648 Days
• Field of Search: 250/341, 250/339.07, 250/339.08, 250/339.12, 250/341.1, 250/341.2, 250/341.8, 250/339.11, 250/340, 356/133, 356/300, 356/436
• US Class Current: 250/339.12
• CPC Class Codes: G01N 21/552 Attenuated total reflection

Abstract

A probe for use in attentuated total reflectance measurements in spectroscopy, such as Fourier transform infrared spectroscopy, is formed of an optical waveguide element having input and output sections and a loop between the two sections. The loop has a small radius of curvature and is exposed so that it can be contacted with a sample to obtain attenuated total reflectance measurements. The input and output sections may be retained in the bore of a thin walled tube with the loop forming a tip which extends from one end of the tube. The input and output sections of the optical waveguide element may be connected by couplers to a spectrometer to receive the output beam from and provide a return beam to the spectrometer. The tightly curved surfaces of the optical waveguide element at the loop result in multiple internal reflections as the beam of radiation traverses the loop. Attenuated total reflectance interactions occur between the beam of radiation and sample material in contact with the loop, which can comprise a liquid, a gas, or relatively soft solid materials.

Claims

1. A probe for use in obtaining attenuated total reflectance measurements comprising:

an optical waveguide element having a diameter of 1 mm or less and an input section, an output section and a loop therein which can be contacted with a sample to obtain attentuated total reflectance measurements, the optical waveguide element formed of an optical material which will transmit electromagnetic radiation of desired wavelengths, the loop being formed to retain a radius of curvature of the loop which is selected relative to the diameter of the waveguide element such that electromagnetic radiation in the optical waveguide element will execute substantially more reflections off the surfaces of the waveguide element in the loop than in the input and output sections adjacent to the loop such that attenuated total reflectance measurements can be obtained when the loop is in contact with a sample material on which the measurements are to be made, and a hollow tube engaging the input and output sections adjacent to the loop to hold them adjacent to one another and extending away from the loop in the same direction, the input and output sections of the optical waveguide element adjacent to the loop passing through a bore of the tube, with the loop extending from a free end of the tube.

2. The probe of claim 1 wherein the loop and the input and output sections of the optical waveguide element adjacent to the loop are free to move in the bore of the tube so that the loop can be withdrawn from the free end of the tube into the bore of the tube.

3. The probe of claim 2 wherein the retaining structure further includes material sealing the loop to the free end of the tube.

4. The probe of claim 1 further including a coupler on an end of each of the input and output sections of the optical waveguide element extending from the loop, the couplers suited for coupling electromagnetic radiation into and out of the optical waveguide element to an optical system.

5. The probe of claim 1 wherein the optical waveguide element is formed of chalcogenide glass.

6. The probe of claim 1 wherein the probe further comprises at least two of said optical waveguide elements with the tube engaging each of the input and output sections adjacent to the loops formed in each of the optical waveguide elements.

7. The probe of claim 1 wherein the free end of the tube is cut at an angle to form a sharpened point adapted to penetrate solid objects.

8. A probe for use in obtaining attenuated total reflectance measurements comprising:

an optical waveguide element having an input section, an output section, and a loop between the input and output sections, the optical waveguide element formed of an optical material which will transmit electromagnetic radiation of desired wavelengths, the loop in the optical waveguide element having its surface exposed to allow attenuated total reflectance measurements and the loop being formed to retain a radius of curvature less than 2 mm; and

an elongated thin walled tube having a hollow bore through which the input and output sections of the optical waveguide element extend adjacent to one another and each section having an end thereof extending out of the tube, the loop extending from a free end of the tube where it may be exposed to the material to be tested.

9. The probe of claim 8 further including a sealing material sealing the free end of the tube adjacent to the loop and providing support for the loop.

10. The probe of claim 9 wherein the material sealing the loop to the free end of the tube is epoxy.

11. The probe of claim 8 further including a coupler on and end of each of the input and output sections of the optical waveguide element extending from the loop, the couplers suited for coupling electromagnetic radiation into and out of the optical waveguide element to an optical system.

12. The probe of claim 8 wherein the optical waveguide element is formed of chalcogenide glass.

13. The probe of claim 8 wherein the optical waveguide element has a diameter less than 1 mm.

14. The probe of claim 8 wherein the probe further comprises at least two of said optical waveguide elements with the loop formed in each of the optical waveguide elements extending from the free end of the tube.

15. The probe of claim 8 wherein the thin walled tube is formed of metal.

16. The probe of claim 8 wherein the free end of the tube is cut at an angle to form a sharpened point adapted to penetrate solid objects.

17. A spectroscopic system comprising:

an infrared spectrometer providing an output beam of infrared radiation and adapted to receive and detect a beam of infrared which has interacted with a sample to affect the spectrum of the radiation in the beam;

a probe for attenuated total reflectance measurements comprising an optical waveguide element having an input section, an output section, and a loop between the input and output sections which can be contacted with a sample to obtain attentuated total reflectance measurements, the optical waveguide element formed of an optical material which will transmit infrared radiation of desired wavelengths, the loop being formed to retain a radius of curvature of the loop which is selected relative to the diameter of the optical waveguide element such that infrared radiation in the optical waveguide element will execute substantially more reflections off the surfaces of the waveguide element in the loop than in the input and output sections of the waveguide element adjacent to the loop such that attenuated total reflectance measurements can be obtained when the loop is in contact with the sample on which the measurements are to be made, and a hollow tube engaging the input and output sections adjacent to the loop to hold them adjacent to one another and extending away from the loop in the same direction, the input and output sections of the optical waveguide element passing through the bore of the tube, with the loop extending from a free end of the tube;

optical coupling cables connected to the spectrometer and the probe to receive the output beam from the spectrometer and direct the beam from the spectrometer to the input section of the optical waveguide element of the probe, and to direct the infrared radiation from the output section of the probe back to the spectrometer.

18. The spectroscopic system of claim 17 wherein the loop and the input and output sections of the optical waveguide element adjacent to the loop are free to move in the bore of the tube so that the loop can be withdrawn from the free end of the tube into the bore of the tube.

19. The spectroscopic system of claim 17 wherein the hollow tube further includes material sealing the loop to the free end of the tube.

20. The spectroscopic system of claim 17 wherein the optical waveguide element of the probe is formed of chalcogenide glass.

21. The spectroscopic system of claim 17 wherein the optical waveguide element has a diameter less than 1 mm, and the radius of curvature of the loop is greater than the diameter of the optical waveguide element and less than 2 mm.

22. The spectroscopic system of claim 17 wherein the probe further comprises at least two of said optical waveguide elements with the tube engaging the input and output sections of each optical waveguide element to support the loop formed in each of the optical waveguide elements.

23. A method of carrying out attenuated total reflectance measurements on a sample, comprising the steps of:

(a) providing an optical waveguide element having an input section, an output section, and a loop between the input and output sections, the loop having a radius of curvature of less than 2 mm and its surface exposed to allow attenuated total reflectance measurements, the optical waveguide element suited for transmitting desired wavelengths of electromagnetic radiation;

(b) providing electromagnetic radiation to the input section of the optical waveguide element having a desired band of wavelengths of electromagnetic radiation and directing the electromagnetic radiation with the optical waveguide element through the loop and returning the electromagnetic radiation passed through the output section of the optical fiber to a spectrometer;

(c) contacting the loop of the optical waveguide element with a localized portion of the sample while passing electromagnetic radiation therethrough to affect the electromagnetic radiation by attenuated total reflectance interaction between the electromagnetic radiation and the sample to obtain measurements by the spectrometer only on the localized portion of the sample contacted by the loop.

24. The method of claim 23 including retaining the input and output sections of the optical waveguide element in the bore of a thin walled tube with the loop formed as a tip extending from one end of the tube.

25. A probe for use in obtaining attenuated total reflectance measurements comprising:

an optical waveguide element having an input section, an output section and a loop therein which can be contacted with a sample to obtain attentuated total reflectance measurements, the optical waveguide element formed of an optical material which will transmit electromagnetic radiation of desired wavelengths, the optical waveguide element in the loop being shaped to taper to a point such that electromagnetic radiation in the optical waveguide element will execute substantially more reflections off the surfaces of the waveguide element in the loop than in the input and output sections adjacent to the loop such that attenuated total reflectance measurements can be obtained when the point of the loop is in contact with a sample material on which the measurements are to be made, and retaining structure engaging the input and output sections adjacent to the loop to hold them adjacent to one another and extending away from the loop in the same direction.

26. The probe of claim 25 wherein the retaining structure comprises a hollow tube, the input and output sections of the optical waveguide adjacent to the loop passing through a bore of the tube, with the loop extending from one end of the tube.

27. The probe of claim 26 wherein the hollow tube further includes material sealing the loop to the one end of the tube.

28. The probe of claim 25 wherein the optical waveguide element is formed of chalcogenide glass.

29. The probe of claim 25 wherein the optical waveguide element has a diameter less than 1 mm.