External/internal optical adapter for FTIR spectrophotometer

• US 8,766,191 B2
• Filed: 10/06/2010
• Issued: 07/01/2014
• Est. Priority Date: 10/06/2009
• Status: Active Grant

• Current Assignee: Curators of the University of Missouri (University of Missouri)
• Original Assignee: Curators of the University of Missouri (University of Missouri)
• Inventors: Xu, Zhi
• Primary Examiner(s): Porta, David
• Assistant Examiner(s): Malevic, Djura
• Application Number:
  US12/898,879
• Publication Number:
  US 20110079718A1
• Time in Patent Office: 1,364 Days
• Field of Search: 250/339.08, 356/433
• US Class Current: 250/339.08
• CPC Class Codes: G01J 3/4535 Devices with moving mirror G01J3/4532 takes precedence

Abstract

A Fourier Transfer Infrared (FTIR) spectrophotometer having reduced baseline noise. The system and method include internal or external optical adapters having a moveable beamsplitter for splitting the source light beam into a reference beam and a sample beam, and may include a variable bandpass filter, variable preamplifier and reversed biased photodiodes.

Claims

1. An adapter for use with an FTIR spectrophotometry system having a light source generating a source light beam of coherent light, said adapter comprising

a sealed housing for receiving the source light beam directed along a propagation path;

an optical system within the housing including a single moveable beamsplitter having first and second reflecting surfaces, each coated with a reflecting layer, said beamsplitter for splitting the source light beam into;

(1) a reference beam reflected by the first reflecting surface to form a first linear path different from the source path, and

(2) a sample beam reflected by the second reflecting surface to form a second linear path different from the source path and different from the first linear path,

wherein the beamsplitter and its first and second reflecting surfaces are moveable together in a direction perpendicular to the propagation path of the source beam between the first and second linear paths to minimize source noise and to minimize a centerburst of a waveform of an interferogram of the reference beam and the sample beam;

a reference cell within the housing, said reference cell including a reference for interacting with the reference beam wherein said interacting yields an output reference beam having a direction;

a reference light detector for detecting at least a portion of the output reference beam based on the direction of the output reference beam and generating a reference signal representative of the detected light;

a sample cell within the housing, said sample cell including a sample for interacting with the sample beam wherein said interacting yields an output sample beam having a direction;

a sample light detector for detecting at least a portion of the output sample beam based on the direction of the output sample beam and generating a sample signal representative of the detected light;

a detector circuit for producing a difference signal proportional to the difference between the reference signal and the sample signal; and

a processor configured to determine a spectrum of the sample based on the difference signal.

2. The adapter of claim 1 wherein the detector circuit includes a variable gain amplifier.

3. The adapter of claim 1 further comprising a variable electronic bandpass filter between the detector circuit and the processor for filtering the difference signal and wherein the processor is configured to determine a spectrum of the sample based on the filtered difference signal.

4. The adapter of claim 3 wherein the spectrophotometry system comprises an FTIR spectrophotometer with a moving mirror and wherein the variable electronic bandpass filter has a variable band center and a variable bandwidth and wherein the band center and the bandwidth are a function of a center wavelength of the optical absorption band, a full width at half maximum (FWHM) bandwidth of the optical absorption band and a speed at which the moving mirror of the FTIR spectrophotometer travels.

5. The adapter of claim 1 further comprising a first phase shifting device for shifting the phase of the reference signal and a second phase shifting device for shifting the phase of the sample signal and wherein the detector circuit produces a reference signal proportional to the phase shifted reference signal and a difference signal proportional to the difference between the phase shifted reference signal and the phase shifted sample signal.

6. The adapter of claim 1 wherein the reference light detector comprises a reference photodiode and the sample light detector comprises a sample photodiode and further comprising a switch selectively electrically connecting a grounded cathode of the reference photodiode and an anode of the sample photodiode and wherein an anode of the reference photodiode is connected to a cathode of the sample photodiode at a point which provides a current signal, and an amplifier converting the current signal into a reference voltage and a difference voltage.

7. The adapter of claim 6 wherein the amplifier has different current-to-voltage conversion factors.

8. The adapter of claim 1 wherein the reference light detector comprises a reference photodiode and the sample light detector comprises a sample photodiode and wherein a cathode of the reference photodiode is electrically connected by a central point to an anode of the sample photodiode, the central point providing a current signal, wherein an anode of the reference photodiode is connected to reverse-biasing battery, wherein a cathode of the sample photodiode is connected to reverse-biasing battery, and an amplifier converting the current signal into a reference voltage and a difference voltage.

9. The adapter of claim 8 wherein the amplifier has different current-to-voltage conversion factors.

10. The adapter of claim 1 wherein the beamsplitter is positioned to minimize a center burst of a waveform of an interferogram with a reference in both the reference cell and the sample cell so that the reference signal and sample signal are balanced and at least some source noise is cancelled in the difference signal.

11. The adapter of claim 1 wherein the detector circuit comprises a circuit for selectively producing a reference voltage proportional to the reference signal and a difference voltage proportional to the difference between the reference signal and the sample signal wherein the beamsplitter is moveable along the first and second paths to a position at which noise cancellation is increased and the signal to noise ratio of the difference signal is increased.

12. The adapter of claim 1 wherein the first linear path is opposite the second linear path and wherein each reflecting layer provides a uniform reflectivity within an infrared region from 700 nm to 10 μ

m.

13. The adapter of claim 1 wherein the beamsplitter is moveable between the first and second linear paths to vary the position of the beamsplitter relative to source light beam, to vary the position of the beamsplitter relative to the reference beam and to vary the position of the beamsplitter relative to the sample beam to minimize source noise including at least one of digitization errors and tracking errors.

14. A method of determining an optical spectrum for a sample substance relative to a reference substance, said method for use with a spectrophotometry system having a light source generating a source light beam of coherent light, said method comprising:

1) splitting, by using a single beamsplitter having first and second reflecting surfaces, each coated with a reflecting layer, the source beam into a reference beam having a path different than the source beam and a sample beam having a path different than the source beam and the reference beam;

2) directing the reference beam into a reference cell having a substance therein, said substance in the reference cell interacting with the reference beam, said interacting yielding an output reference beam having a direction;

3) directing the sample beam into a sample cell having a substance therein, said substance in the sample cell interacting with the sample beam, said interacting yielding an output sample beam having a direction;

4) detecting at least a portion of the output reference beam and at least a portion of the output sample beam;

5) generating a reference signal representative of the detected portion of the output reference beam and a sample signal representative of the detected portion of the output sample beam;

6) generating a difference signal proportional to the difference between the reference signal and the sample signal;

7) placing the reference substance in the reference cell and in the sample cell;

8) determining a reference spectrum of the reference substance based on the difference signal;

9) moving the beamsplitter in a direction perpendicular to the propagation of the source beam to determine a minimized noise location of the beamsplitter at which a center burst of an interferogram is minimized;

10) determining a baseline difference spectrum;

11) placing the beamsplitter at the determined minimized noise location by moving the beamsplitter and its first and second reflecting surfaces together in a direction perpendicular to the propagation path of the source beam between the first and second linear paths;

12) thereafter placing the reference substance in the reference cell and placing the sample substance in the sample cell;

13) determining a sample difference spectrum; and

14) determining the absorption spectrum of the sample based on the reference spectrum, the baseline difference spectrum and the sample difference spectrum.

15. The method of claim 14 further comprising shifting the phase of the reference signal, shifting the phase of the sample signal, producing a reference voltage proportional to the phase shifted reference signal and producing a difference voltage proportional to the difference between the phase shifted reference signal and the phase shifted sample signal.

16. The method of claim 14 wherein the spectrophotometry system comprises an FTIR spectrophotometer with a moving mirror and wherein a variable bandpass filter filters the difference signal, said filter having a variable band center and a variable bandwidth and further comprising setting the band center and the bandwidth of the filter as a function of a center wavelength of the optical absorption band, a full width at half maximum (FWHM) bandwidth of the optical absorption band and a speed at which the moving mirror of the FTIR spectrophotometer travels.

17. A spectrophotometry system comprising:

a light source generating a light beam;

a lens in a path of the light beam and transmitting the light beam as a coherent source light beam;

an optical system within the housing including a single moveable beamsplitter having first and second reflecting surfaces, each coated with a reflecting layer, said beamsplitter for splitting the source light beam into;

(1) a reference beam reflected by the first reflecting surface to form a first linear path different from the source path, and

(2) a sample beam reflected by the second reflecting surface to form a second linear path different from the source path and different from the first linear path,

wherein the beamsplitter and its first and second reflecting surfaces are moveable together in a direction perpendicular to the propagation path of the source beam between the first and second linear paths;

a reference cell including a reference for interacting with the reference beam wherein said interacting yields an output reference beam having a direction;

a reference light detector for detecting at least a portion of the output reference beam based on the direction of the output reference beam and generating a reference signal representative of the detected light;

a sample cell including a sample for interacting with the sample beam wherein said interacting yields an output sample beam having a direction;

a sample light detector for detecting at least a portion of the output sample beam based on the direction of the output sample beam and generating a sample signal representative of the detected light;

a detector circuit for producing a difference signal proportional to the difference between the reference signal and the sample signal;

a sealed housing for enclosing the light source, the lens, the optical system including the moveable beamsplitter, the reference cell including the reference, the reference light detector, the sample cell including the sample, the sample light detector, and the detector circuit; and

a processor configured to determine a spectrum of the sample based on the difference signal configured to determine and minimize a centerburst of a waveform of an interferogram of the reference beam and the sample beam.

18. The system of claim 17 wherein the detector circuit includes a variable gain amplifier.

19. The system of claim 17 further comprising a variable electronic bandpass filter between the detector circuit and the processor for filtering the difference signal and wherein the processor is configured to determine a spectrum of the sample based on the filtered difference signal.

20. The system of claim 19 wherein the spectrophotometry system comprises an FTIR spectrophotometer with a moving mirror and wherein the variable electronic bandpass filter has a variable band center and a variable bandwidth and wherein the band center and the bandwidth are a function of a center wavelength of the optical absorption band, a full width at half maximum (FWHM) bandwidth of the optical absorption band and a speed at which the moving mirror of the FTIR spectrophotometer travels.

21. The system of claim 17 further comprising a first phase shifting device for shifting the phase of the reference signal and a second phase shifting device for shifting the phase of the sample signal and wherein the detector circuit produces a reference signal proportional to the phase shifted reference signal and a difference signal proportional to the difference between the phase shifted reference signal and the phase shifted sample signal.

22. The system of claim 17 wherein the reference light detector comprises a reference photodiode and the sample light detector comprises a sample photodiode and further comprising a switch selectively electrically connecting a grounded cathode of the reference photodiode and an anode of the sample photodiode and wherein an anode of the reference photodiode is connected to a cathode of the sample photodiode at a point which provides a current signal, and an amplifier converting the current signal into a reference voltage and a difference voltage.

23. The system of claim 22 wherein the amplifier has different current-to-voltage conversion factors.

24. The system of claim 17 wherein the reference light detector comprises a reference photodiode and the sample light detector comprises a sample photodiode and wherein a cathode of the reference photodiode is electrically connected by a central point to an anode of the sample photodiode, the central point providing a current signal, wherein an anode of the reference photodiode is connected to reverse-biasing battery, wherein a cathode of the sample photodiode is connected to reverse-biasing battery, and an amplifier converting the current signal into a reference voltage and a difference voltage.

25. The system of claim 24 wherein the amplifier has different current-to-voltage conversion factors.

26. The system of claim 17 wherein the beamsplitter is positioned to minimize a center burst of a waveform of an interferogram with a reference in both the reference cell and the sample cell so that the reference signal and sample signal are balanced and at least some source noise is cancelled in the difference signal.

27. The system of claim 17 wherein the detector circuit comprises a circuit for selectively producing a reference voltage proportional to the reference signal and a difference voltage proportional to the difference between the reference signal and the sample signal wherein the beamsplitter is moveable along the first and second paths to a position at which noise cancellation is increased and the signal to noise ratio of the difference signal is increased.