Parallel infrared spectroscopy apparatus and method
원문보기
IPC분류정보
국가/구분
United States(US) Patent
등록
국제특허분류(IPC7판)
G01J-003/10
G01J-003/00
G01K-011/00
G01K-013/02
G01K-013/00
G01K-025/00
G01N-031/00
출원번호
US-0900612
(2004-07-28)
등록번호
US-7255474
(2007-08-14)
발명자
/ 주소
Cong,Peijun
Guan,Shenheng
Cypes,Stephen
Wells,Jason
Bergh,H. Sam
출원인 / 주소
Symyx Technologies, Inc.
인용정보
피인용 횟수 :
12인용 특허 :
48
초록▼
A library of material samples is provided in a condition suitable for imaging using infrared (IR) spectroscopy. The samples are provided to one or more detection cells, each of the cells including or containing a reflective surface. Preferably, for imaging, an energy source (e.g. a source of infrare
A library of material samples is provided in a condition suitable for imaging using infrared (IR) spectroscopy. The samples are provided to one or more detection cells, each of the cells including or containing a reflective surface. Preferably, for imaging, an energy source (e.g. a source of infrared radiation) provides energy to the detection cells to interact with the samples. Thereafter, images (e.g., spectra) related to the samples are created based upon the interaction.
대표청구항▼
We claim: 1. An apparatus for simultaneously evaluating flow reactions comprising a parallel infrared detection system for simultaneously analyzing at least two flowing fluid samples, comprising: a parallel flow reactor comprising two or more reactors, each of the two or more reactors comprising a
We claim: 1. An apparatus for simultaneously evaluating flow reactions comprising a parallel infrared detection system for simultaneously analyzing at least two flowing fluid samples, comprising: a parallel flow reactor comprising two or more reactors, each of the two or more reactors comprising a reaction cavity for carrying out a chemical reaction, an inlet port in fluid communication with the reaction cavity for providing a feed stream comprising one or more reactants to the reaction cavity, and an outlet port in fluid communication with the reaction cavity for discharging an effluent stream comprising one or more reaction products, and a fluid distribution system comprising a feed distribution subsystem for simultaneously supplying the feed stream to the inlet port of each of the two or more reactors, and an effluent distribution subsystem for discharging the effluent stream from the outlet port of each of the two or more reactors, the parallel infrared detection system comprising (a) at least two detection cells, each of the at least two detection cells comprising (i) a detection cavity having one or more infrared reflective surfaces for reflecting infrared radiation, (ii) an inlet port for receiving one of the at least two samples into the detection cavity, and (iii) an outlet port for discharging the sample from the detection cavity; (b) one or more infrared radiation sources for simultaneously irradiating each of the at least two samples with infrared radiation in the detection cavity of their respective detection cells, the one or more infrared radiation sources and the one or more infrared reflective surfaces being configured such that infrared radiation reflects off of the one or more infrared reflective surfaces within the detection cavity of each of the detection cells; and (c) a detector configured for simultaneously detecting reflected infrared radiation from each of the detection cells over time for analysis of the samples, wherein the effluent distribution subsystem of the parallel flow reactor is configured such that at least a portion of the discharged effluent steam of one of the two or more reactors is provided as a flowing fluid sample to the inlet port of a respective one of the detection cells. 2. An apparatus as in claim 1 wherein the one or more reflective surfaces are formed of a broadband IR reflective material. 3. An apparatus as in claim 2 wherein the reflective material is selected from gold, silver or a metal halide. 4. An apparatus as in claim 1 wherein the at least two detection cells includes at least four detection cells. 5. An apparatus as in claim 4 wherein the at least four detection cells includes at least 16 detection cells. 6. An apparatus as in claim 1 wherein the detection system has a detection limit below about 1000 ppm. 7. An apparatus as in claim 1 wherein the detection system has a detection limit below about 100 ppm. 8. An apparatus as in claim 1 wherein the one or more infrared reflective surfaces include a reflective end surface. 9. An apparatus as in claim 8 wherein the reflective end surface is proximate to the inlet port. 10. An apparatus as in claim 1 wherein the one or more infrared reflective surfaces include a waveguide. 11. An apparatus as in claim 1 wherein the one or more infrared reflective surfaces include a waveguide and a reflective end surface. 12. An apparatus comprising a parallel infrared detection system for simultaneously analyzing at least two flowing fluid samples, the detection system comprising (a) at least two detection cells, each of the at least two detection cells comprising (i) an elongated detection cavity comprising a first end, a second end defined by an infrared-transparent window, and an elongated side surface between the first end and the second end, the elongated side surface being effective for guiding an infrared wave of radiation along the elongated cavity, (ii) an inlet port for receiving one of the at least two samples into the detection cavity, and (iii) an outlet port for discharging the sample from the detection cavity, (b) one or more infrared radiation sources for simultaneously irradiating each of the at least two samples with infrared radiation in the detection cavity of their respective detection cells, the one or more infrared radiation sources being configured to provide Incident infrared radiation through the infrared-transparent window of each detection cavity such that the incident infrared radiation interacts with the sample in the respective detection cavity, and (c) a detector configured for simultaneously detecting infrared radiation from each of the detection cells over time for analysis of the samples, wherein the at least two detection cells are configured in relative relation to each other to have a first-end pitch defined by the center-to-center distance between adjacent detection cavities at the first end thereof, and a second-end pitch defined by the center-to-center distance between adjacent detection cavities at the second end thereof, the first-end pitch of the at least two detection cells being greater than the second-end pitch of the at least two detection cells. 13. The apparatus of claim 12 wherein for each of the at least two detection cells, at least a portion of the elongated detection cavity is non-linear, the non-linear portion of the elongated detection cavity comprising a non-linear elongated side surface. 14. The apparatus of claim 12 wherein for each of the at least two detection cells, the outlet port is positioned proximate to the infrared transparent window. 15. The apparatus of claim 12 wherein for each of the at least two detection cells, the outlet port is defined by a spaced relationship between an open end of the elongated side surface and the infrared transparent window. 16. An apparatus comprising a parallel infrared detection system for simultaneously analyzing at least two flowing fluid samples, the detection system comprising (a) at least two detection cells, each of the at least two detection cells comprising (i) an elongated detection cavity comprising a first end, a second end defined by an infrared-transparent window, and an elongated side surface between the first end and the second end, the elongated side surface being effective for guiding an infrared wave of radiation along the elongated cavity, (ii) an inlet port for receiving one of the at least two samples into the detection cavity, and (iii) an outlet port for discharging the sample from the detection cavity, (b) one or more infrared radiation sources for simultaneously irradiating each of the at least two samples with infrared radiation in the detection cavity of their respective detection cells, the one or more infrared radiation sources being configured to provide incident infrared radiation trough the infrared-transparent window of each detection cavity such that the incident infrared radiation interacts with the sample in the respective detection cavity, (c) a detector configured for simultaneously detecting infrared radiation from each of the detection cells over time for analysis of the samples, and a pressure chamber in fluid communication with the outlet port of each of the at least two detection cells. 17. The apparatus of claim 16 wherein the pressure chamber is adapted for operating conditions comprising a pressure of at least about 100 psig and for a temperature of at least about 100째 C. 18. The apparatus of claim 16 further comprising a pressure regulator for regulating the pressure in the pressure chamber. 19. The apparatus of claim 16 wherein the pressure chamber includes a sweep system comprising a sweep gas source, an inlet port in fluid communication with the sweep gas source for admitting the sweep gas into the pressure chamber, an outlet port for discharging the sweep gas out of the pressure chamber, and a pressure regulator for regulating the pressure in the pressure chamber. 20. The apparatus of claim 12 wherein the detector comprises a focal plane array comprising at least eight pixels, the focal plane ray and the detection cells being configured, such that (i) for each of the at least two detection cells, infrared radiation is received from the detection cell into at least four pixels of the focal plane array, and (ii) at least about 50% of the total number of pixels of the focal plane array receive reflected infrared radiation from a detection cell. 21. The apparatus of claim 12 wherein the first end of the elongated detection cavity is defined by an infrared-reflective end surface for reflecting infrared radiation. 22. The apparatus of claim 12 wherein the first end of the elongated detection cavity is defined by an infrared-reflective end surface for reflecting infrared radiation, and the detector is configured for simultaneously receiving infrared radiation from each of the detection cells through the infrared transparent window. 23. An apparatus comprising a parallel infrared detection system for simultaneously analyzing at least two flowing fluid samples, the detection system comprising (a) at least two detection cells, each of the at least two detection cells comprising (i) an elongated detection cavity comprising a first end defined by an infrared-reflective end surface for reflecting infrared radiation, a second end defined by an infrared-transparent window, and an elongated side surface between the first end and the second end, the elongated side surface being defined at least partially by a capillary waveguide, at least a portion of the elongated detection cavity being non-linear, (ii) an inlet port for receiving one of the at least two samples into the detection cavity, and (iii) an outlet port for discharging the sample from the detection cavity, the at least two detection cells being configured in relative relation to each other to have a first-end pitch defined by the center-to-center distance between adjacent detection cavities at the first end thereof, and a second-end pitch defined by the center-to-center distance between adjacent detection cavities at the second end thereof, the first-end pitch of the at least two detection cells being greater than the second-end pitch of the at least two detection cells (b) one or more infrared radiation sources for simultaneously irradiating each of the at least two samples with infrared radiation in the detection cavity of their respective detection cells, the one or more infrared radiation sources being configured to provide incident infrared radiation through the infrared-transparent window of each detection cavity such that the incident infrared radiation interacts with the sample in the respective detection cavity, and (c) a detector comprising a focal plane array and being configured for simultaneously detecting infrared radiation from each of the detection cells over time for analysis of the samples, the focal plane array and the detection cells being configured, such that (i) for each of the at least two detection cells, infrared radiation is received from the detection cell into at least four pixels of the focal plane array, and (ii) at least about 50% of the total number of pixels of the focal plane array receive reflected infrared radiation from a detection cell. 24. An apparatus, for simultaneously evaluating flow reactions comprising a parallel infrared detection system for simultaneously analyzing at least two flowing fluid samples, comprising a parallel flow reactor comprising two or more reactors, each of the two or more reactors comprising a reaction cavity for carrying out a chemical reaction, an inlet port in fluid communication with the reaction cavity for providing a feed stream comprising one or more reactants to the reaction cavity, and an outlet port in fluid communication with the reaction cavity for discharging an effluent stream comprising one or more reaction products, and a fluid distribution system comprising a feed distribution subsystem for simultaneously supplying the feed stream to the inlet port of each of the two or more reactors, and an effluent distribution subsystem for discharging the effluent stream from the outlet port of each of the two or more reactors, the parallel infrared detection system comprising (a) at least two detection cells, each of the at least two detection cells comprising (i) an elongated detection cavity comprising a first end, a second end defined by an infrared-transparent window, and an elongated side surface between the first end and the second end, (ii) an inlet port for receiving one of the at least two samples into the detection cavity, and (iii) an outlet port for discharging the sample from the detection cavity, (b) one or more infrared radiation sources for simultaneously irradiating each of the at least two samples with infrared radiation in the detection cavity of their respective detection cells, the one or more infrared radiation sources being configured to provide incident infrared radiation through the infrared-transparent window of each detection cavity such that the incident infrared radiation interacts with the sample in the respective detection cavity; and (c) one or more detectors configured for simultaneously detecting infrared radiation from each of the detection cells over time for analysis of the samples; wherein each of the detection cavities, the one or more infrared sources, the infrared-transparent window of each detection cavity, and the one or more detectors are configured such that the detection system has a detection limit below about 100 ppm, and wherein the effluent distribution subsystem of the parallel flow reactor is configured such that at least a portion of the discharged effluent stream of one of the two or more reactors is provided as a flowing fluid sample to the inlet port of a respective one of the detection cells. 25. An apparatus as in any of claims 1, 12, 16, 23 or 24 further comprising a processor for performing Fourier transform infrared analysis on the reflected infrared radiation or images thereof. 26. An apparatus as in claim 25 wherein the processor performs the Fourier transform infrared analysis simultaneously for the at least two samples. 27. A method for simultaneously analyzing at least two flowing fluid samples using parallel infrared detection, the method comprising: providing a parallel flow reactor comprising two or more reactors, each of the two or more reactors comprising a reaction cavity, an inlet port in fluid communication with the reaction cavity and an outlet port in fluid communication with the reaction cavity; providing a fluid distribution system comprising a feed distribution subsystem and an effluent distribution subsystem; providing at least two detection cells, each of the at least two detection cells comprising (i) a detection cavity having one or more infrared reflective surfaces for reflecting infrared radiation, (ii) an inlet port for receiving one of the at least two samples into the detection cavity, and (iii) an outlet port for discharging the sample from the detection cavity; simultaneously feeding a reactant stream comprising one or more reactants through the inlet port of each of the two or more reactors to the reaction cavity of each of the two or more reactors, simultaneously contacting the one or more reactants with a catalyst in the reaction cavity under reaction conditions to form one or more reaction products; discharging the one or more reaction products from the reaction cavity of each of the reactors as an effluent stream through the outlet port of each of the reaction cavities to the effluent distribution subsystem of the fluid distribution system; providing at least a portion of the discharged effluent stream from each of the reactors to the inlet port of each of the detection cells as the at least two fluid samples; simultaneously flowing the at least two fluid samples respectively through the inlet port of each of the detection cells into the detection cavity; simultaneously directing infrared radiation through an infrared transparent window into the detection cavity of each of the detection cells such that the infrared radiation reflects off of the one or more infrared reflective surfaces within the detection cavity of each of the detection cells and respectively interacts with each of the at least two samples for simultaneously irradiating the at least two samples with reflected infrared radiation; simultaneously detecting the reflected infrared radiation from each of the detection cells over time for analysis of the samples; and simultaneously flowing the at least two fluid samples respectively out of the detection cavity of each of the detection cells through the outlet port of each of the detection cells. 28. A method as in claim 27 wherein the one or more reflective surfaces are formed of a broadband IR reflective material. 29. A method as in claim 27 wherein the one or more reflective surfaces are formed from a material selected from gold, silver or a metal halide. 30. A method as in claim 27 wherein the at least two detection cells includes at least four detection cells. 31. A method as in claim 27 wherein the at least two detection cells includes at least 16 detection cells. 32. A method as in claim 27 wherein the detection system has a detection limit below about 1000 ppm. 33. A method as in claim 27 wherein the detection system has a detection limit below about 100 ppm. 34. A method as in claim 27 wherein the one or more infrared reflective surfaces includes a reflective end surface that is proximate to the inlet port. 35. A method as in claim 27 wherein the at least two samples are reaction products of different reactions. 36. A method of performing parallel infrared detection for simultaneously analyzing at least two flowing fluid samples, the method comprising: providing at least two detection cells, each of the at least two detection cells comprising (i) an elongated detection cavity comprising a first end, a second end defined by an infrared-transparent window, and an elongated side surface between the first end and the second end, (ii) an inlet port for receiving one of the at least two samples into the detection cavity, and (iii) an outlet port for discharging the sample from the detection cavity; flowing the at least two fluid samples respectively through the inlet port of each of the detection cells into the detection cavity; directing infrared radiation through an infrared transparent window into the detection cavity of each of the detection cells such that the elongated side surface reflects and guides the infrared radiation along the elongated cavity to respectively interact with each of the at least two samples for simultaneously irradiating the at least two samples with reflected infrared radiation; detecting the reflected infrared radiation from each of the at least two detection cells over time for analysis of the samples; and flowing the at least two fluid samples respectively out of the detection cavity of each of the at least two detection cells via the outlet port of each of the at least two detection cells, wherein the at least two detection cells are configured in relative relation to each other to have a first-end pitch defined by the center-to-center distance between adjacent detection cavities at the first end thereof, and a second-end pitch defined by the center-to-center distance between adjacent detection cavities at the second end thereof, the first-end pitch of the at least two detection cells being greater than the second-end pitch of the at least two detection cells. 37. The method of claim 36 wherein for each of the at least two detection cells, at least a portion of the elongated detection cavity is non-linear, the non-linear portion of the elongated detection cavity comprising a non-linear elongated side surface. 38. The method of claim 36 wherein for each of the at least two detection cells, the outlet port is positioned proximate to the infrared transparent window. 39. The method of claim 36 wherein for each of the at least two detection cells, the outlet port is defined by a spaced relationship between an open end of the elongated side surface and the infrared transparent window. 40. A The method of claim 36 wherein the at least two fluid samples flow out of the detection cavity into a common pressure chamber in fluid communication with the outlet port of each of the at least two detection cells. 41. The method of claim 40 wherein the pressure chamber is adapted for operating conditions comprising a pressure of at least about 100 psig and for a temperature of at least about 100째 C. 42. The method of claim 40 further comprising regulating the pressure in the pressure chamber. 43. The method of claim 40 further comprising sweeping the pressure chamber with a sweep gas to reduce cross-contamination between fluid samples in adjacent detection cells. 44. The method of claim 36 wherein the detector comprises a focal plane array comprising at least eight pixels, and (i) for each of the at least two detection cells, the reflected infrared radiation from the detection cell is received into at least four pixels of the focal plane array, and (ii) at least about 50% of the total number of pixels of the focal plane array receive reflected infrared radiation from a detection cell. 45. The method of claim 36 wherein the first end of the elongated detection cavity is defined by an infrared-reflective end surface for reflecting infrared radiation. 46. The method of claim 36 wherein the first end of the elongated detection cavity is defined by an infrared-reflective end surface for reflecting infrared radiation, and the detector is configured for simultaneously receiving infrared radiation from each of the detection cells through the infrared transparent window. 47. A method of performing parallel infrared detection for simultaneously analyzing at least two flowing fluid samples, the method comprising: providing a parallel flow reactor comprising two or more reactors, each of the two or more reactors comprising a reaction cavity, an inlet port in fluid communication with the reaction cavity and an outlet port in fluid communication with the reaction cavity; providing a fluid distribution system comprising a feed distribution subsystem and an effluent distribution subsystem; providing at least two detection cells, each of the at least two detection cells comprising (i) a detection cavity having one or more infrared reflective surfaces for reflecting infrared radiation, (ii) an inlet port for receiving one of the at least two samples into the detection cavity, and (iii) an outlet port for discharging the sample from the detection cavity; simultaneously feeding a reactant stream comprising one or more reactants through the inlet port of each of the two or more reactors to the reaction cavity of each of the two or more reactors, simultaneously contacting the one or more reactants with a catalyst in the reaction cavity under reaction conditions to form one or more reaction products; discharging the one or more reaction products from the reaction cavity of each of the reactors as an effluent stream trough the outlet port of each of the reaction cavities to the effluent distribution subsystem of the fluid distribution system; providing at least a portion of the discharged effluent stream from each of the reactors to the inlet port of each of the detection cells as the at least two fluid samples; flowing the at least two fluid samples respectively through the inlet port of each of the detection cells into the detection cavity; directing infrared radiation through an infrared transparent window into the detection cavity of each of the detection cells such that the infrared radiation reflects off of the one or more infrared reflective surfaces within the detection cavity of each of the detection cells and respectively interacts with each of the at least two samples for simultaneously irradiating the at least two samples with reflected infrared radiation; detecting the reflected infrared radiation from each of the detection cells over time with a detection limit below about 100 ppm for one or more components of each of the samples; and flowing the at least two fluid samples respectively out of the detection cavity of each of the detection cells via the outlet port of each of the detection cells. 48. A method as in any of claims 27, 36, or 47 further comprising, performing Fourier transform infrared analysis upon the reflected infrared radiation or images thereof. 49. A method of claim 48 wherein the step of performing Fourier transform infrared analysis is carried out simultaneously for the at least two samples.
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