CALIBRATION VERIFICATION FOR OPTICAL PARTICLE ANALYZERS

20210404936

17/290494

April 27, 2020

Provided are particle analyzers and related methods for verifying calibration status of the particle analyzer, including independently of the presence or absence of particles. The method and analyzers include use of distinct and non-interfering time frequency domains: a middle frequency time domain and a low frequency time domain, and optionally a high frequency time domain. The high frequency time domain generates a laser facet drive current frequency modulation to prevent the laser facet from spatial-mode hopping. The middle frequency time domain is for particle detection. The low frequency time domain is for calibration status, including laser-pulse-light self-diagnostics, for the health or calibration status of the analyzer. By carefully selecting the frequency time domain ranges, there is non-interference, with the ability to self-diagnose the instrument that is particle-independent.

Particle Measuring Systems, Inc. (Boulder, CO, US)

1. A method for determining a calibration status of an optical particle analyzer independent of particles, the method comprising the steps of: providing an optical particle analyzer including: a source of electromagnetic radiation (EMR) for generating a beam of said EMR; a chamber for containing a sample medium and for receiving said beam of EMR; an optical assembly in optical communication with the source of EMR for directing the beam of EMR from to the chamber; a detector for detecting scattered radiation from said beam of EMR; an optical collection system for directing said scattered radiation from the beam of EMR from the chamber and to the detector; modulating a power applied to the source of EMR; in response to the modulating step, inducing a detector signal waveform having a low frequency time domain; analyzing the detector signal waveform to determine a value of at least one diagnostic parameter associated with one or more of the source of EMR, the optical assembly, the chamber, the detector, and the optical collection system; determining the calibration status of the optical particle analyzer based on the one or more determined values of the at least one diagnostic parameter; wherein for one or more particles present in the optical particle analyzer and in response to the step of modulating the power applied to the source of EMR a particle detection signal is generated having a middle frequency time domain that is higher than the low frequency time domain, thereby avoiding unwanted interference between the low frequency time domain of the detector signal and the middle frequency time domain of the particle detection signal; thereby determining the calibration status of an optical particle analyzer independent of particles.

2. The method of claim 1, wherein said source of EMR is a laser.

3. The method of claim 2, further comprising the step of: applying a high frequency time domain laser facet drive current frequency to modulate a current applied to the laser at a high-frequency time domain to prevent spatial mode hopping; wherein the high frequency time domain is of a higher frequency than the middle frequency time domain and does not interfere with any of the middle frequency or low frequency time domains.

4. The method of any of claims 1-3, wherein: the high frequency time domain is greater than or equal to 100 MHz, including about 249 MHz; the middle frequency time domain is selected from a range that is between 1 kHz/7 kHz and 200 MHz; and/or the low frequency time domain range is less than or equal to 500 Hz.

5. The method of any of claims 1-4, wherein the one or more particles in the optical particle analyzer is from: residual contamination of the analyzer; and/or from a particle in a sample that is being analyzed by the optical particle analyzer simultaneously with the determining the calibration status.

6. The method of claim 1, wherein the calibration status is determined in the presence of particles interacting with the beam of EMR.

7. The method of claims 1-6, further comprising the step of filtering the particle detection system with a low band-pass filter and a high band-pass filter to obtain the middle frequency time domain.

8. The method of any of claims 1-7, wherein the chamber comprises a flow chamber.

9. The method of any of claims 1-8, wherein the sample medium is a fluid, said method further comprising flowing the fluid through the flow chamber during the modulating step.

10. The method of claim 9, wherein the flowing step comprises filtering the fluid upstream of the flow chamber.

11. The method of any of claims 1-10, wherein the sample medium includes particles.

12. The method of any of claims 1-11, wherein the modulating step further comprises switching the power applied to the source of EMR from a first power level to a second power level.

13. The method of claim 12, wherein the switching step further comprises switching the power applied to the source of EMR according to a switching waveform having a frequency, a duty cycle, a first switching amplitude corresponding to the first power level, and a second switching amplitude corresponding to the second power level.

14. The method of any of claims 1-13, further comprising maintaining the power applied to the source of EMR at a second power level for a time selected over the range of 1 ms to 1 s.

15. The method of any of claims 1-14, wherein the inducing step includes: first receiving, by the detector, the scattered radiation from said beam of EMR or said laser beam at a first radiant power level corresponding to a first power level applied to the source of EMR; and second receiving, by the detector, the scattered radiation from said beam of EMR or said laser beam at a second radiant power level corresponding to a second power level applied to the source of EMR; and wherein the detector signal waveform has: a leading edge; a first signal amplitude; and a second signal amplitude.

16. The method of claim 15, wherein the leading edge of the detector signal waveform is defined by a leading edge function.

17. The method of any of claims 15-16, wherein the optical particle analyzer further includes amplification circuitry operably connected to the detector for amplifying a detector signal in response to the inducing step, and wherein the second receiving step includes changing an energization state of the amplification circuitry from a first state to a second state corresponding to the first and second radiant power levels, respectively.

18. The method of claim 17, wherein the leading edge of the detector signal waveform corresponds to the change of the energization state of the amplification circuitry from the first state to the second state.

19. The method of any of claims 17-18, wherein the at least one diagnostic parameter is further associated with the amplification circuitry.

20. The method of any of claims 15-19, wherein the at least one diagnostic parameter includes a detector signal waveform peak amplitude defined as a value of a difference between a value of the first signal amplitude and a value of the second signal amplitude value, and wherein the analyzing step further comprises determining: the value of the first signal amplitude; the value of the second signal amplitude; and the value of the difference between the first and second amplitude values.

21. The method of claim 20, wherein the optical particle analyzer further includes amplification circuitry operably connected to the detector for amplifying a detector signal in response to the inducing step, and wherein the detector signal waveform peak amplitude is associated with an operational condition of the source of EMR, the chamber, the optical assembly, the optical collection system, the detector, and the amplification circuitry.

22. The method of any of claims 15-21, wherein the at least one diagnostic parameter includes an elapsed time for the leading edge, and wherein the analyzing step includes determining the elapsed time for the leading edge.

23. The method of claim 22, wherein the optical particle analyzer further includes drive circuitry for the source of EMR, and wherein the elapsed time for the leading edge is associated with an operational condition of the drive circuitry.

24. The method of claim 16, wherein the at least one diagnostic parameter includes the leading edge function, and wherein the analyzing step includes determining the leading edge function of the leading edge.

25. The method of claim 24, wherein the leading edge function is associated with an operational condition of the source of EMR, the optical assembly, the chamber, the detector, and the optical collection system of the optical particle analyzer.

26. The method of any of claims 1-25, wherein the determining step further comprises comparing the one or more determined values of the at least one diagnostic parameter with corresponding values of at least one of the respective calibration parameter determined at a prior calibration of the optical particle analyzer.

27. The method of claim 26, wherein the comparing step includes determining a difference between the one or more determined values of the at least one diagnostic parameter and the corresponding values of each respective calibration parameter determined at the prior calibration.

28. The method of claim 27, wherein the step of determining the calibration status comprises determining the calibration status of the optical particle analyzer based on the determined difference.

29. An optical particle analyzer comprising: a source of EMR for generating a beam of said EMR; a chamber for containing a sample medium and for receiving said beam of EMR; an optical assembly in optical communication with the source of EMR for directing the beam of EMR from the source of EMR to the chamber; a detector for detecting scattered radiation from said beam of EMR; an optical collection system for directing scattered radiation from the beam of EMR from the chamber and to the detector; and a processor operably connected to the source of EMR and the detector, wherein the processor is programmed to: modulate a power applied to the source of EMR from a first power level to a second power level; analyze a scattered radiation detector signal waveform induced by the modulation of the power applied to the source of EMR at a low frequency time domain; determine a value of at least one diagnostic parameter from the scattered radiation detector signal waveform associated with one or more of the source of EMR, the chamber, the optical assembly, the detector, and the optical collection system, determine a calibration status of the optical particle analyzer based on the one or more determined values of the at least one diagnostic parameter; and for one or more particles present in the optical particle analyzer and in response to the modulate the power a particle detection signal is generated having a middle frequency time domain that is higher than the low frequency time domain, thereby avoiding unwanted interference between the low frequency time domain and the middle frequency time domain so that the determined diagnostic parameter status is independent of presence or absence of particles in the chamber.

30. The optical particle analyzer of claim 29, further comprising: a low band-pass filter and a high band-pass filter each electronically connected to the detector to obtain the middle frequency time domain.

31. The optical particle analyzer of any of claims 29-30, wherein the chamber comprises a flow chamber.

32. The optical particle analyzer of any of claims 29-31, wherein the sample medium is a fluid, and wherein the optical particle analyzer further comprises a flow system for flowing the fluid through the flow chamber.

33. The optical particle analyzer of claim 32, further comprising a filter for filtering the fluid upstream of the flow chamber.

34. The optical particle analyzer of any of claims 29-33, wherein the sample medium includes particles.

35. The optical particle analyzer of any of claims 29-34, wherein, to modulate the power applied to the source of EMR, the processor is further programmed to switch the power applied to the source of EMR from a first power level to a second power level.

36. The optical particle analyzer of claim 35, wherein, to switch the power applied to the source of EMR, the processor is further programmed to switch the power applied to the source of EMR according to a switching waveform having a frequency, a duty cycle, a first switching amplitude corresponding to the first power level, and a second switching amplitude corresponding to the second power level.

37. The optical particle analyzer of any of claims 29-36, wherein the processor is further programmed to maintain the power applied to the source of EMR at a second power level for a time selected over the range of 1 ms to 1 s.

38. The optical particle analyzer of any of claims 29-37, wherein, in response to the scattered radiation detector signal waveform induced by the modulation of the power applied to the source of EMR, the processor is further programmed to: first receive a first detector signal from the detector, the first detector signal representative of scattered radiation from said beam of EMR at a first radiant power level corresponding to the first power level applied to the source of EMR; and second receive a second detector signal from the detector, the second detector signal representative of scattered radiation from said beam of EMR at a second radiant power level corresponding to the second power level applied to the source of EMR; and wherein the scattered radiation detector signal waveform has: a leading edge; a first signal amplitude; and a second signal amplitude.

39. The optical particle analyzer of claim 38, wherein the leading edge of the scattered radiation detector signal waveform is defined by a leading edge function.

40. The optical particle analyzer of any of claims 38-39, further comprising amplification circuitry operably connected to the detector for amplifying the first and second detector signals prior to receipt by the processor, and wherein, in response to the modulation of the power applied to the source of EMR, an energization state of the amplification circuitry changes from a first state to a second state corresponding to the first and second radiant power levels, respectively.

41. The optical particle analyzer of claim 40, wherein the leading edge of the scattered radiation detector signal waveform corresponds to the change of the energization state of the amplification circuitry from the first state to the second state.

42. The optical particle analyzer of any of claims 40-41, wherein the at least one diagnostic parameter is further associated with the amplification circuitry.

43. The optical particle analyzer of any of claims 38-42, wherein the at least one diagnostic parameter includes a scattered radiation detector signal waveform peak amplitude defined as a value of a difference between a value of the first signal amplitude and a value of the second signal amplitude value, and wherein, to analyze the scattered radiation detector signal waveform induced by the modulation of the power applied to the source of EMR, the processor is further programmed to determine: the value of the first signal amplitude; the value of the second signal amplitude; and the value of the difference between the first and second amplitude values.

44. The optical particle analyzer of claim 43, further comprising amplification circuitry operably connected to the detector for amplifying the first and second detector signals prior to receipt by the processor, wherein the scattered radiation detector signal waveform peak amplitude is associated with an operational condition of the source of EMR, the chamber, the optical assembly, the optical collection system, the detector, and the amplification circuitry.

45. The optical particle analyzer of any of claims 38-44, wherein the at least one diagnostic parameter includes an elapsed time for the leading edge, and wherein, to analyze the scattered radiation detector signal waveform induced by the modulation of the power applied to the source of EMR, the processor is further programmed to determine the elapsed time for the leading edge.

46. The optical particle analyzer of claim 45, further comprising drive circuitry for the source of EMR, wherein the elapsed time for the leading edge is associated with an operational condition of the drive circuitry.

47. The optical particle analyzer of claim 39, wherein the at least one diagnostic parameter includes the leading edge function, and wherein, to analyze the scattered radiation detector signal waveform induced by the modulation of the power applied to the source of EMR, the processor is further programmed to determine the leading edge function of the leading edge.

48. The optical particle analyzer of claim 47, wherein the leading edge function is associated with an operational condition of the source of EMR, the optical assembly, the chamber, the detector, and the optical collection system of the optical particle analyzer.

49. The optical particle analyzer of any of claims 29-48, wherein, to determine the value of at least one diagnostic parameter, the processor is further programmed to compare the one or more determined values of the at least one diagnostic parameter with corresponding values of at least one of the respective calibration parameter determined at a prior calibration of the optical particle analyzer.

50. The optical particle analyzer of claim 49, wherein, to compare the one or more determined values of the at least one diagnostic parameter with the corresponding values of at least one of the respective calibration parameter determined at the prior calibration of the optical particle analyzer, the processor is further programmed to determine a difference between the one or more determined values of the at least one diagnostic parameter and the corresponding values of each respective calibration parameter determined at the prior calibration.

51. The optical particle analyzer of claim 50, wherein the processor is further programmed to determine the calibration status of the optical particle analyzer based on the determined difference.

52. The optical particle analyzer of claim 29, wherein the source of EMR includes at least one of a laser, a diode laser, a strip diode laser, a light emitting diode, and an incandescent lamp.

53. The optical particle analyzer of claim 29, wherein the source of EMR is a laser and at least one diagnostic parameter includes an amplitude of a peak of the scattered radiation detector signal waveform corresponding to a difference in detector signal amplitudes between: the scattered radiation detected by the detector from the laser beam at a first radiant power level from the laser having the applied power at the first power level; and the scattered radiation detected by the detector from the laser beam at a second radiant power level from the laser having the applied power at the second power level.

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