WO2002097407A1 - Procede de detection optique d'especes chimiques contenues dans les milieux condenses - Google Patents
Procede de detection optique d'especes chimiques contenues dans les milieux condenses Download PDFInfo
- Publication number
- WO2002097407A1 WO2002097407A1 PCT/FR2002/001832 FR0201832W WO02097407A1 WO 2002097407 A1 WO2002097407 A1 WO 2002097407A1 FR 0201832 W FR0201832 W FR 0201832W WO 02097407 A1 WO02097407 A1 WO 02097407A1
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- WO
- WIPO (PCT)
- Prior art keywords
- chemical species
- electromagnetic
- backscattered
- determined
- wavelength
- Prior art date
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/645—Specially adapted constructive features of fluorimeters
- G01N21/6456—Spatial resolved fluorescence measurements; Imaging
Definitions
- the present invention relates to a method and a device for detecting chemical species present in a condensed medium.
- Fields of applications envisaged are in particular those of controlling the composition of aqueous effluents escaping from a water treatment plant or from any industry discharging effluents.
- Another field of application envisaged is that of controlling the formation of a chemical compound in an industrial production process.
- control of industrial discharges in nature, in liquid form is generally carried out visually and by analysis of samples of liquid discharged according to a methodology specific to each chemical species sought.
- aqueous effluent which may contain chemical species which are not uniformly distributed over said area, it is necessary to take several samples at different locations in order to locate the origin of the production of said area. species.
- the time required for the analysis of the sample and the speed of movement of said effluent affect the diagnosis as to this location.
- the detection of the appearance of a reaction compound by taking samples from the reaction medium has a double disadvantage.
- the reaction is affected by the taking of said sample, and then, the longer the time necessary for the analysis of said chemical compound in front of the reaction speed and the less control of the reaction is possible.
- the electromagnetic excitation means directed towards the medium to be analyzed, excite a surface of the medium.
- the incident signal must be large enough to excite all the species of the surface and on the other hand, the detection means must be extremely sensitive to detect the spectra of said chemical species of said surface.
- a problem which arises and which the present invention aims to solve is then to propose a method for detecting chemical species present in a condensed medium which not only makes it possible to precisely detect the nature of the chemical species present in said condensed medium with means less expensive detection, but also, which allows to excite the surface of said condensed medium with reduced power means and therefore also inexpensive.
- the present invention provides a method for detecting chemical species comprising the following steps: determining, the wavelengths and the intensity values characteristic of electromagnetic emission signals backscattered in response to a plurality electromagnetic excitations, of different wavelengths, of at least one chemical species capable of being contained in said condensed medium; successively exciting a plurality of surface elements of a surface portion of said condensed medium, with a beam of laser means whose tunable wavelength is capable of taking at least the values of said wavelengths distinct from said plurality electromagnetic excitations; the wavelengths and the intensity values of electromagnetic emission signals backscattered by each of said surface elements are recorded successively in response to the electromagnetic excitations produced by said beam; comparing, at least one excitation wavelength and at least one corresponding emission wavelength, the value intensity, recorded, of said electromagnetic signal backscattered by each of said surface elements at said characteristic value, determined, of said electromagnetic signal backscattered from said chemical species likely to be contained in said surface portion; and, the presence of said chemical species in each of said surface elements is determined when said recorded
- the method resides in the analysis of the backscattered electromagnetic signals, due to the fluorescence of the chemical species excited by a beam, coming from laser means, said signals being characteristic of said chemical species.
- the targeted chemical species diffuse electromagnetic signals whose intensities and wavelengths are characteristic of said species. In this way, by exciting a specific chemical species with laser means and by varying the excitation frequency, backscattered signals are obtained, the wavelengths and intensities of which are characteristic.
- the method according to the invention makes it possible to detect the presence of said chemical species given on a more or less extended portion of the surface of the condensed medium by decomposing said surface portion into surface elements and by exciting said surface element with a laser beam at said determined incident wavelengths and by comparing the lengths and the intensities of the backscattered signals recorded at wavelengths and at the intensities characteristic of the signals of said species.
- the bundle of laser means is capable of being applied directly to the surface of the condensed medium and its intersection with said surface determines said surface element.
- the threshold value is adjusted as a function of the noise level of the detector system.
- the surface elements of the entire surface portion are capable of being analyzed independently of each other with good precision since the laser beam is concentrated on a surface element of a surface portion and that is recorded. the wavelengths and the intensity values of the signals backscattered by said surface element. In this way, the power of the laser means can be reduced and the detection means be less sensitive while retaining good detection.
- the compounds of the surface elements are successively excited and for each surface element, the wavelength of the incident radiation is varied and the backscattered signals are collected so as to establish the presence or not of the chemical species determined in all the surface elements of said surface portion.
- a chemical species is capable of presenting several characteristic emission signals at different wavelengths in response to a single excitation wavelength.
- the incident radiation will be granted on this excitation wavelength only if only this chemical species is sought.
- the direction of said beam of the laser means is recorded successively for each surface element of said surface portion so as to identify the source of said backscattered electromagnetic emission signals, whereby the position of said chemical species in said surface portion.
- the distance which separates the laser means from the surface portion being known, the relative positions of each surface element are determined by the relative angular deviations of the direction of the beam if the laser means pivots around a fixed point.
- said back-broadcast electromagnetic emission signals corresponding to this surface element are assigned so as to identify the position of said chemical species.
- the concentration of said chemical species present in said medium is further determined by measuring the amount of energy emitted by said electromagnetic emission signals backscattered.
- the energy of the backscattered signal is a function of the number of photons emitted and therefore a function of the quantity of the chemical species which diffuses the incident radiation, it is possible, after calibration, to correlate the energy of the backscattered signal and the quantity of said chemical species.
- the intensity values of said backscattered electromagnetic emission signals are recorded in parallel and their corresponding wavelength is recorded.
- the spectra of the chemical species present in the surface portion are recorded at a high speed.
- the position and the intensity of said signal are detected by the detector means simultaneously with the measurement of the wavelength of said signal.
- the presence of the chemical species and its position in the surface portion are determined.
- a second object of the present invention is to provide a device for detecting chemical species present in a condensed medium, comprising: means for determining, the wavelengths and the intensity values characteristic of electromagnetic signals of retro emission - diffused in response to a plurality of electromagnetic excitations, of distinct wavelengths, of at least one chemical species capable of being contained in said condensed medium; laser means producing a beam for successively exciting a plurality of surface elements of a surface portion of said condensed medium according to wavelengths capable of taking at least the values of said wavelengths distinct from said plurality of excitations electromagnetic; means for successively recording the wavelengths and the intensity values of electromagnetic emission signals backscattered by each of said surface elements in response to the electromagnetic excitations produced by said beam; and, comparison and determination means, for comparing with at least one excitation wavelength and at least one corresponding emission wavelength, the intensity value, recorded, of said backscattered electromagnetic signal by each of said surface elements at said determined characteristic intensity value of said backscattered electromagnetic signal of said chemical species capable of being contained in said condensed
- a characteristic of the device lies in the combination of the production means using a coherent electromagnetic beam oriented towards a surface element of said surface portion, at values of determined wavelength and means for recording the intensity and wavelength values of the backscattered signals, these means being in turn combined with the comparison and determination means, which compare said recorded values with the determined values wavelength and intensity of the chemical species likely to be contained in the condensed medium to determine the presence or not of said species.
- said laser means comprise: a pump laser associated with a frequency doubler; and, a parametric oscillator to which said pump laser is coupled so as to emit radiation of which the tunable wavelength . is between 200 and 800 nm.
- said laser means producing a beam comprise, means for orienting said beam to excite said plurality of surface elements of said surface portion of said condensed medium so as to analyze the electromagnetic emission signals backscattered from each of said surface elements and determining the presence of at least one of said chemical species in each of said surface elements of said surface portion.
- the displacement means comprise movable mirrors for orienting the beam on each of the surface elements, these displacement means being controlled by control means.
- the device comprises means for successively recording the direction of said beam of the laser means for each surface element of said portion surface so as to identify the source of said back-broadcast electromagnetic emission signals, whereby the position of said chemical species in said surface portion is obtained.
- the detection device comprises means for recording comprising a spectrometer coupled to a matrix of photodetectors, so as to record in parallel the intensity values of said back-emitted electromagnetic emission signals and to record their length d 'corresponding wave.
- FIG. 2 is a representation of a spectrum capable of being obtained by means of the device according to the invention.
- Figure 1 illustrates the detection device according to the invention, which has laser means 10 forming an excitation beam 12, means 14 for recording a backscattered signal 16 and comparison and determination means 18 contained in the central unit of a computer 20.
- the central unit comprises programs for controlling the entire device according to the invention.
- the laser means 10 comprise a pulsed laser 22 of the "NdYAG" type coupled to a set of frequency converters 24, for example frequency doublers and triplers whose first beam 26 which emerges is oriented towards an optical parametric oscillator 28 making it possible to provide at least one second beam 30 which is directed towards a second frequency doubler 32.
- the parametric oscillator 28 makes it possible to continuously vary the wavelength of the second beam 30.
- said laser means comprise a pumping source operating in femtosecond mode and forming a compact system.
- the tunable laser means 10 make it possible to provide an excitation beam 12 of a section of a few cm 2 at a distance of 100 m and whose wavelength is likely to vary at least between 220 and 750 nm, range of lengths wave in which the chemical species liable to be excited exhibit characteristic spectra.
- the pump laser 22 can advantageously be replaced by a diode system which has the same advantages.
- the excitation beam 12, coming from said laser means 10 passes through semi-transparent means 34, for example a prism or a semi-transparent blade, and then meets means 36 for moving the excitation beam 12 made up of two orientable mirrors , which reflect the beam towards a condensed medium 38 capable of containing chemical compounds.
- semi-transparent means 34 for example a prism or a semi-transparent blade
- means 36 for moving the excitation beam 12 made up of two orientable mirrors which reflect the beam towards a condensed medium 38 capable of containing chemical compounds.
- the intersection of the excitation beam and the surface of the condensed medium forms at about 100 m distance a surface element of a few cm 2 , for example 3 cm 2 .
- Said chemical compounds are capable of emitting a backscattered electromagnetic signal 16 in response to the excitation caused by the excitation beam 12, said backscattered electromagnetic signal 16 imprints the same optical path as the excitation beam 12 up to 'to the transparent means 34 which directs the backscattered signal 16 to the means 14 for recording it.
- These means 14 comprise a spectrometer 40 capable of determining the wavelengths of the backscattered electromagnetic signals 16 and coupled to detector means 42 consisting of a matrix of sensors photoelectric, for example CCD, capable of determining the intensities at a position of the backscattered signals 16.
- the means for recording 14 are connected to the central unit of the computer 20 which has a memory capable of storing simultaneously, in particular, the wavelength of the backscattered signal 16 and its intensity.
- the central unit of the computer 20 is also connected to the laser means 10 and to the means 36 for moving the excitation beam 12, so as to control them by means of the control programs.
- the direction of the excitation beam 12 which determines the position of an excited surface element is also stored in the memory of the computer 20 simultaneously with the intensities and the wavelengths of the backscattered signals.
- the position of the surface elements is capable of being determined by the identification of the pixels of the matrix of photoelectric sensors which are arranged in the focal plane of the optical system.
- the computer 20 can control, for a determined position of the means 36 for moving the excitation beam 12, the laser means 10 so as to vary the wavelength of the excitation beam as a function of time. 12, for example between 250 and 450 nm.
- the computer 20 stores in its memory space, the determined position of the backscattered signal 16, determined by the beam moving means 36, the wavelength and the intensity of the backscattered signal 16 for each of the wavelength values of the excitation beam 12.
- the control programs control the movement of the displacement means 36 so that the excitation beam 12 targets the surface element of the surface portion 38, contiguous to the previous one to carry out the same spectral scanning. This operation is repeated so as to cover the entire surface portion 38.
- five variables are stored in the memory space of the computer 20; three variables characterize chemical species present in the surface element that the excitation beam 12 excites, and two variables characterize the position of said surface element relative to the other surface elements identified by the relative positions of the displacement means 36 and stored in the memory of the computer 20.
- FIG. 2 illustrating the spectra of a mixture containing at least two aromatic hydrocarbons; anthracene and a benzo pyrene.
- Curve 54 represents the intensity of the backscattered signals and their wavelengths in response to an excitation whose wavelength is 380 nm.
- Curve 54 has three vertices 56, 58, 60 respectively at 411 nm, 432 nm and 457 nm, characteristic of benzo pyrene.
- Curve 62 in response to excitation at 390 nm, also has three vertices, 64, 66, 68 at 450, 425 and 396 nm respectively characteristic of anthracene.
- the excitation at 400 nm generates a substantially flat curve 70 allowing no characterization.
- the detection of a given chemical species, anthracene for example, in a determined condensed medium is capable of being carried out by comparing the intensity of the retro signal. diffused at 411, 432 and 457 nm for an excitation produced at 390 nm and by determining the presence of anthracene if for example, the intensity of the signals at all these wavelengths is proportional to the intensity of the signals characteristic of anthracene.
- the spectra of the chemical species, concretized by the intensity and the wavelength of emission of the signals backscattered in response to the excitation signals are determined either by calculation or, preferably, by experience and are stored in databases in the memory of the computer 20.
- anthracene it is not necessary to compare the whole spectrum, which forms a determined surface in space, excitation wavelength, emission wavelength and intensity of the signal emitted, to determine the presence of the chemical species considered, but simply to choose judiciously the wavelengths characteristic of excitation / emission and to compare the intensity of the emission signals.
- the identification of a specific chemical species can be carried out by comparing the spectrum recorded with the spectrum of said chemical species stored in the databases by means of any known identification program.
- a characteristic of the device according to the invention resides in the sequential archiving, surface element by surface element, indexed by the displacement means 36 and stored in the memory of the computer 20, measurements of intensity and wavelength of backscattered signals.
- the three variables are recorded with two location variables characterized by the relative directions of the beam of the laser means.
- Each chemical species has different fluorescence lifetimes. Thus, by collecting the fluorescence emission at well-determined times after the excitation, the interference between the fluorescence signal and the emissive phenomena with very short time is minimized.
- the intensity of fluorescence of each species is measured after a certain delay and for a determined duration, after synchronization of the excitation signal and the detector.
- the intensity values characteristic of electromagnetic emission signals backscattered are determined, in response to an excitation after a determined delay and during a determined time of at least one chemical species capable of being contained in said condensed medium; the intensity values of the backscattered electromagnetic emission signals are recorded, in response to an excitation of said condensed medium after said determined time and during said determined time; and, comparing said recorded intensity values and said determined intensity values so as to determine the presence of said chemical species in said condensed medium.
- the temporal resolution of the fluorescence signal makes it possible to discriminate the different chemical species as a function of the lifetime of their fluorescence emission.
- the detection device according to the invention is capable of being installed above watercourses or rivers into which manufacturers discharge their effluents, in order to continuously monitor the nature of the effluents discharged and whether the chemical species toxic substances that they are likely to produce are not directly released into the environment.
- the optical system placed between the recording means, in particular the detector, and the condensed medium to be explored is completely different when a portion of surface is visualized whose dimensions are of the order of a hundred meters or when we explore a portion of the surface of a living cell.
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- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
Description
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Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP20020748920 EP1393048A1 (fr) | 2001-06-01 | 2002-05-31 | Procede de detection optique d'especes chimiques contenues dans les milieux condenses |
JP2003500538A JP2004527767A (ja) | 2001-06-01 | 2002-05-31 | 濃縮媒質に含まれる化学種の光学検出方法 |
CA002449251A CA2449251A1 (fr) | 2001-06-01 | 2002-05-31 | Procede de detection optique d'especes chimiques contenues dans les milieux condenses |
US10/725,125 US6903817B2 (en) | 2001-06-01 | 2003-12-01 | Method for optically detecting chemical species contained in condensed media |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR0107216A FR2825468B1 (fr) | 2001-06-01 | 2001-06-01 | Procede de detection optique d'especes chimiques contenues dans les milieux condenses |
FR01/07216 | 2001-06-01 |
Related Child Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US10/725,125 Continuation US6903817B2 (en) | 2001-06-01 | 2003-12-01 | Method for optically detecting chemical species contained in condensed media |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2002097407A1 true WO2002097407A1 (fr) | 2002-12-05 |
Family
ID=8863877
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/FR2002/001832 WO2002097407A1 (fr) | 2001-06-01 | 2002-05-31 | Procede de detection optique d'especes chimiques contenues dans les milieux condenses |
Country Status (6)
Country | Link |
---|---|
US (1) | US6903817B2 (fr) |
EP (1) | EP1393048A1 (fr) |
JP (1) | JP2004527767A (fr) |
CA (1) | CA2449251A1 (fr) |
FR (1) | FR2825468B1 (fr) |
WO (1) | WO2002097407A1 (fr) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2005001451A2 (fr) * | 2003-02-24 | 2005-01-06 | Cdex, Inc. | Systeme et procedes de detection et d'identification de substances chimiques |
JP2006507503A (ja) * | 2002-11-21 | 2006-03-02 | シーデックス, インコーポレイテッド | 紫外蛍光を使用して、分子種を検出し、検査し、分類するための方法および装置 |
US7381972B1 (en) | 2006-07-24 | 2008-06-03 | Science Applications International Corporation | System and method for light fluorescence detection |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7106826B2 (en) * | 2002-01-07 | 2006-09-12 | Cdex, Inc. | System and method for adapting a software control in an operating environment |
US10386232B2 (en) | 2017-12-15 | 2019-08-20 | Horiba Instruments Incorporated | Compact spectroscopic optical instrument |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0324583A2 (fr) * | 1988-01-12 | 1989-07-19 | World Geoscience Corporation Limited | Dispositif de détection à distance |
EP0474264A2 (fr) * | 1991-04-24 | 1992-03-11 | Kaman Aerospace Corporation | Méthode et appareil pour l'imagerie à LIDAR spectralement dispersif |
WO1997011355A1 (fr) * | 1995-09-19 | 1997-03-27 | Cornell Research Foundation, Inc. | Microscopie laser multiphotonique |
-
2001
- 2001-06-01 FR FR0107216A patent/FR2825468B1/fr not_active Expired - Fee Related
-
2002
- 2002-05-31 EP EP20020748920 patent/EP1393048A1/fr not_active Ceased
- 2002-05-31 WO PCT/FR2002/001832 patent/WO2002097407A1/fr active Application Filing
- 2002-05-31 JP JP2003500538A patent/JP2004527767A/ja active Pending
- 2002-05-31 CA CA002449251A patent/CA2449251A1/fr not_active Abandoned
-
2003
- 2003-12-01 US US10/725,125 patent/US6903817B2/en not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0324583A2 (fr) * | 1988-01-12 | 1989-07-19 | World Geoscience Corporation Limited | Dispositif de détection à distance |
EP0474264A2 (fr) * | 1991-04-24 | 1992-03-11 | Kaman Aerospace Corporation | Méthode et appareil pour l'imagerie à LIDAR spectralement dispersif |
WO1997011355A1 (fr) * | 1995-09-19 | 1997-03-27 | Cornell Research Foundation, Inc. | Microscopie laser multiphotonique |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006507503A (ja) * | 2002-11-21 | 2006-03-02 | シーデックス, インコーポレイテッド | 紫外蛍光を使用して、分子種を検出し、検査し、分類するための方法および装置 |
US7154102B2 (en) | 2002-11-21 | 2006-12-26 | Cdex, Inc. | System and methods for detection and identification of chemical substances |
WO2005001451A2 (fr) * | 2003-02-24 | 2005-01-06 | Cdex, Inc. | Systeme et procedes de detection et d'identification de substances chimiques |
WO2005001451A3 (fr) * | 2003-02-24 | 2005-03-17 | Cdex Inc | Systeme et procedes de detection et d'identification de substances chimiques |
US7381972B1 (en) | 2006-07-24 | 2008-06-03 | Science Applications International Corporation | System and method for light fluorescence detection |
US7468520B1 (en) | 2006-07-24 | 2008-12-23 | Science Applications International Corporation | System and method for light induced fluorescence detection |
Also Published As
Publication number | Publication date |
---|---|
FR2825468B1 (fr) | 2004-03-19 |
FR2825468A1 (fr) | 2002-12-06 |
US6903817B2 (en) | 2005-06-07 |
JP2004527767A (ja) | 2004-09-09 |
CA2449251A1 (fr) | 2002-12-05 |
US20040135999A1 (en) | 2004-07-15 |
EP1393048A1 (fr) | 2004-03-03 |
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