Robust spectroscopic optical probe

• US 5,657,404 A
• Filed: 05/25/1995
• Issued: 08/12/1997
• Est. Priority Date: 05/25/1995
• Status: Expired due to Fees

• Current Assignee: Rosemount Analytical, Inc. (Emerson Electric Company)
• Original Assignee: Eastman Chemical Company
• Inventors: Edwards, Roger Dale, Buchanan, Norma Lindsey, Nelson, Gregory Wayne, Nicely, Vincent Alvin, Alsmeyer, Daniel Charles
• Primary Examiner(s): Lee, John D.
• Application Number:
  US08/450,597
• Time in Patent Office: 810 Days
• Field of Search: 356/246, 356/300, 356/301, 356/317, 356/318, 356/432, 356/436, 356/440, 385/12, 385/15, 385/31, 385/39, 385/138, 385/139, 385/902
• US Class Current: 385/12
• CPC Class Codes: G01N 21/8507 Probe photometers, i.e. with optical measuring part dipped into fluid sample
• CPC Class Codes: G02B 6/241 Light guide terminations
• CPC Class Codes: G02B 6/3855 characterised by the method of anchoring or fixing the fibre within the ferrule G02B6/3854 takes precedence

Abstract

Disclosed is a spectroscopic probe apparatus useful for Raman, near infrared, luminescence, ultraviolet or visible spectroscopies that is formed with a robust method of construction using a molten metal soldering technique. The disclosed method and apparatus provides an optical probe that is easy to manufacture yet able to withstand drastic environmental conditions without damage and produce useful spectroscopic results under such conditions.

Claims

1. A fluid-tight spectroscopic optical probe comprising:

(a) a fluid-tight housing;

(b) a probe tip having a terminal surface, said probe tip sealably closing one end of said housing;

(c) at least one fiber optic excitation channel terminating at said terminal surface of said probe tip and extending within the length of said housing, said excitation channel transmitting radiation from a radiation source to a chemical composition to be irradiated for spectroscopic analysis; and

(d) at least one fiber optic collection channel terminating at said terminal surface of said probe tip and extending within the length of said housing, said collection channel transmitting radiation from an irradiated chemical composition to detector means remotely situated from said chemical composition;

wherein said fiber optic excitation channel and said fiber optic collection channel are each separated from one another and securely held and sealed within said probe tip by solder means encompassing each said channel.

2. The probe of claim 1 comprising two to six fiber optic collection channels.

3. The probe of claim 1 comprising two to six fiber optical excitation channels.

4. The probe of claim 1 wherein said housing and tip are formed from solder-adherable metal.

5. The probe of claim 4 wherein said metal is stainless steel.

6. The probe of claim 1 wherein said excitation channel and said collection channel each comprises an optical fiber having a circular cross-section, said fibers having a diameter of 1 μ

m to 1000 μ

m.

7. The probe of claim 6 wherein said diameter is 200 μ

m to 400 μ

m.

8. The probe of claim 6 wherein each said optical fiber further comprises a peripheral surface bearing a thin solder-adherable metallic layer.

9. The probe of claim 8 wherein said metallic layer comprises gold.

10. The probe of claim 6 wherein each said optical fiber comprises a step-indexed multimode optical fiber.

11. The probe of claim 1 wherein said solder means comprises a solder plug, said plug being situated at said terminal surface of said tip.

12. The probe of claim 11 wherein said solder plug is formed of a silver solder or a gold solder.

13. The probe of claim 1 further comprising a reflector cap that includes a concave mirror, said cap being situated in close proximity to said tip and capable of reflecting radiation from said excitation channel to said collection channel.

14. The probe of claim 1 wherein said detector means comprises a spectrometer.

15. The probe of claim 14 wherein said spectrometer is an ultraviolet-visible (UV/VIS) spectrometer, a near infrared (NIR) spectrometer, a Raman spectrometer, or a luminescence spectrometer.

16. The probe of claim 15 wherein said spectrometer is a Raman spectrometer and said radiation source is a laser.

17. The probe of claim 16 wherein said laser is a diode laser.

18. The probe of claim 15 wherein said spectrometer is a near infrared (NIR) spectrometer and said radiation source is a halogen-modified tungsten lamp.

19. The probe of claim 15 wherein said spectrometer is an ultraviolet-visible (UV-VIS) spectrometer and said radiation source is a tungsten lamp.

20. The probe of claim 1 comprising a single fiber optic excitation channel.

21. The probe of claim 1 comprising a single fiber optic collection channel.

22. A method for forming a fluid-tight spectroscopic optical probe provided with a fluid-tight housing and a probe tip having a terminal surface and sealably closing one end of said housing, said housing and said probe tip each being formed of solder-adherable metal;

at least one excitation channel that transmits radiation from a radiation source to a chemical composition to be irradiated; and

at least one collection channel that transmits radiation from an irradiated chemical composition to detector means remotely situated from said chemical composition, each said channel comprising an optical fiber having a circular cross-section, one end of each said fiber terminating at said terminal surface of said probe tip and extending within the length of said housing;

said method comprising;

forming a cavity at said terminal surface of said probe tip;

filling said cavity with molten metal solder, then allowing said solder to cool and solidify to a plug;

forming at least two closely spaced holes of circular cross-section penetrating through said plug, said holes having a cross-section very slightly larger than the cross-section of said optical fibers;

inserting one end of each of said optical fibers through said probe tip and into each of said holes in said plug, thereby substantially filling said holes in said probe tip and plug, said ends of said fibers being separated from one another and together with said plug forming a substantially continuous surface with said terminal surface of said probe tip;

heating said solder plug to a temperature sufficient to cause the solder to flow around and encompassing each said optical fiber end;

cooling said plug to ambient temperature, thereby securing and sealing said separated optical fiber ends at said terminal surface of said probe tip; and

grinding and polishing said substantially continuous terminal surface of said probe tip, thereby forming an optically smooth terminal surface.

23. The method of claim 22 wherein said solder plug is formed of a silver solder or a gold solder.

24. The method of claim 22 further comprising:

sealably connecting said housing with said probe tip by soldering.

25. The method of claim 22 wherein each said optical fiber further comprises a peripheral surface bearing a thin solder-adherable layer of gold.

26. The method of claim 22 wherein each said optical fiber has a diameter of about 200 μ

m to 400 μ

m.