WO2012018299A1 - Spectrograph for short wavelength detection in gas chromatography - uv detection - Google Patents

Spectrograph for short wavelength detection in gas chromatography - uv detection Download PDF

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Publication number
WO2012018299A1
WO2012018299A1 PCT/SE2011/050970 SE2011050970W WO2012018299A1 WO 2012018299 A1 WO2012018299 A1 WO 2012018299A1 SE 2011050970 W SE2011050970 W SE 2011050970W WO 2012018299 A1 WO2012018299 A1 WO 2012018299A1
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WO
WIPO (PCT)
Prior art keywords
spectrograph
gas
light
slit
substances
Prior art date
Application number
PCT/SE2011/050970
Other languages
French (fr)
Inventor
Lennart Olsson
Hans Verner Lagesson
Original Assignee
Chromalytica Ab
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Chromalytica Ab filed Critical Chromalytica Ab
Publication of WO2012018299A1 publication Critical patent/WO2012018299A1/en

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/74—Optical detectors
    • 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
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/15—Preventing contamination of the components of the optical system or obstruction of the light path
    • 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
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/02—Details
    • G01J3/04—Slit arrangements slit adjustment
    • 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
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/15—Preventing contamination of the components of the optical system or obstruction of the light path
    • G01N2021/151—Gas blown
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/74—Optical detectors
    • G01N2030/746—Optical detectors detecting along the line of flow, e.g. axial

Definitions

  • the present invention relates Gas Chromatography, GC - Ultraviolet absorption, UV - spectroscopy, GC-UV, to detect, identify and analyse gases, liquids and solid unknown substances from high to very low
  • the basic technology is known and used for various purposes.
  • the invention relates to physical, mechanical and software control solutions.
  • the invention solves one of the major problems to achieve in order to detect absorption of very short wavelengths (typically down to 120nm) for identification of unknown substances in gas phase.
  • the invention is very versatile and can be used in various applications such as hand held portable and laboratory based bench top instruments.
  • One particular use is for detection of metabolic or other substances emanating from living cells, tissues and in particular that can be found in exhaled air, saliva, sweat, blood and urine from humans, animals, organisms and plants etc. for detection of various deceases and metabolic activities such as stress.
  • Substances can be such as nitrogen oxide, urea, acetone, isoprene, carbon disulphide coming from diseases like gastric ulcers, asthma, diabetes, psychiatric disorders, drug abuse, stress conditions and intoxications, etc.
  • Gas chromatography UV - spectroscopy is used for identification and quantification of various substances that can be transformed into gas.
  • the technology is based on that substances in gas phase first passes through a heated column where the gas has a substance dependent velocity through the column and when the gas to be analysed leaves the first heated column and enters a chamber where UV light passes the gas, absorb light when the light passes the gas, in a spectral way, so the photonic spectrum relates with very high accuracy to the identity of the substance.
  • the light used for the absorption shall preferably have a broad spectrum of wavelengths to allow absorption over a broad spectrum of wavelengths.
  • the passage, chamber, where light penetrates the gas shall be designed to have the gas absorb as much light as possible and to achieve maximum resolution in the analyse, the chamber volume shall be kept as small as possible.
  • the process is basically a gas chromatography where a chamber with a light path is added in the end of the column so the gas passes through the chamber and absorbs light with a spectrum that is related to the gas.
  • the remaining lights then passes into a spectrograph and further on to a light sensitive sectioned array preferably a CCD, Charge Coupled Device, so the spatial light components hits individual light sensitive elements enabling spatial detection of the light and thereby allows identification of the substance to be analysed.
  • a light sensitive sectioned array preferably a CCD, Charge Coupled Device
  • Light is directed in to the spectrograph trough a passage that can be a window made out of a photon transparent material that allow passage of the required wavelengths.
  • Materials used in such windows can be made of MgF2 or material with similar optical properties with the drawback like of being sensitive to rapid
  • Any physical window acts as a filter of passing photons in particular for short wavelength photons. It is also important to keep the spectrograph, its dispersive element and photon sensitive array clean from contamination like particles and residuals from gases, like sublimated matter from gas in order to keep the functionality of the spectrograph.
  • a physical window has to be cleaned or replaced regularly due to
  • An object of the present invention is to eliminate at least one of the drawbacks mentioned above, which is achieved by assigning to the characteristics according to claim 1- 8.
  • the light entrance to the spectrograph is not provided with a physical solid barrier like a physical window, but prevention of gas to be analysed to enter the spectrograph is made by flow of inert gas like nitrogen or other gases out from the
  • spectrograph trough light entrance slit of the spectrograph.
  • Different pressure at the different locations directs the flow of gas in a desired way from locations with higher pressure to locations with lower pressure. If the gas pressure in the spectrograph is kept higher than outside, the gas flow from the spectrograph passes out through the slit and there will be an efficient barrier against intrusion of gas, still with the ability for short wavelength light to pass through from outside into the spectrograph..
  • the light entrance to the spectrograph is not provided with a physical solid barrier like a physical window, but preventing the amount of gas to be analysed to enter the spectrograph can be made by having the entrance slit so small that the undesired entrance of gas from outside into the spectrograph is of minor importance for the function.
  • Fig. 1 shows schematically a device in accordance with a first embodiment of the invention
  • Fig. 2 shows schematically a device in accordance with a second
  • the invention relates to a method of increasing the transparency of very short wavelength photons in GC-UV applications.
  • Fig. 1 shows schematically a spectrometer (9) comprising a spectrograph (8) with a dispersive element (1 ) with light beams (3, 5) passing through a small slit (7) and reflects at the dispersive element (1 ) and hits a light sensitive element (2) like a CCD (2).
  • a gas supplying means (not shown) is provided for producing gas flows (4) into the spectrograph and then out of the spectrograph trough a slit (7).
  • the pressure of the gas decline from where it enters (4) the spectrograph to where then the gas exit from the spectrograph trough the slit (7).
  • the drop of pressure over the slit (7) creates a velocity of the gas that prevents gas or particles to enter through the slit (7) in the reverse direction.
  • the spectrograph - spectrometer does not comprise a physical window, but only a dynamic gas flow that does not filter any of the light (5) that enters through the slit (7) the full spectrum of incoming lights (5) will enter the spectrograph - spectrometer.
  • Fig. 2 shows schematically a spectrometer (9) comprising a spectrograph (8) with a dispersive element (1 ) with light beams (3, 5) passing through a slit (7) and reflects at the dispersive element (1 ) and hits a light sensitive element (2) like a CCD (2).
  • the slit (7) is so small that the flow of gas from outside the spectrograph into the same is so small that it will only marginally affect the function of the spectrograph and spectrometer.
  • a spectrograph is consisting of a slit (7) where light enters, a dispersive element that reflects the fractioned light.
  • a spectrometer is a spectrograph that has a photon collecting device (2) to collect the fractioned light (10) for read out and measurement of spectra.
  • the Photon collecting device can be a CCD - Charge Collecting Device (2).

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

A method and a solution in a gas chromatography –UV spectrography detector to efficiently increase the flow of photons through the spectrograph to a light sensitive element or elements and maintain functionality despite the absence of a physical window for the light to enter the spectrograph.

Description

SPECTROGRAPH FOR SHORT WAVELENGTH DETECTION IN GAS CHROMATOGRAPHY - UV DETECTION.
TECHNICAL FIELD The present invention relates Gas Chromatography, GC - Ultraviolet absorption, UV - spectroscopy, GC-UV, to detect, identify and analyse gases, liquids and solid unknown substances from high to very low
concentrations. The basic technology is known and used for various purposes. The invention relates to physical, mechanical and software control solutions. The invention solves one of the major problems to achieve in order to detect absorption of very short wavelengths (typically down to 120nm) for identification of unknown substances in gas phase.
The invention is very versatile and can be used in various applications such as hand held portable and laboratory based bench top instruments. One particular use is for detection of metabolic or other substances emanating from living cells, tissues and in particular that can be found in exhaled air, saliva, sweat, blood and urine from humans, animals, organisms and plants etc. for detection of various deceases and metabolic activities such as stress. Substances can be such as nitrogen oxide, urea, acetone, isoprene, carbon disulphide coming from diseases like gastric ulcers, asthma, diabetes, psychiatric disorders, drug abuse, stress conditions and intoxications, etc.
Many of those metabolic substances have significant high absorption of UV light in a spectrum ranging from about 120 nm wave length and longer.
BACKGROUND ART
Gas chromatography UV - spectroscopy is used for identification and quantification of various substances that can be transformed into gas. The technology is based on that substances in gas phase first passes through a heated column where the gas has a substance dependent velocity through the column and when the gas to be analysed leaves the first heated column and enters a chamber where UV light passes the gas, absorb light when the light passes the gas, in a spectral way, so the photonic spectrum relates with very high accuracy to the identity of the substance.
The light used for the absorption shall preferably have a broad spectrum of wavelengths to allow absorption over a broad spectrum of wavelengths. The passage, chamber, where light penetrates the gas shall be designed to have the gas absorb as much light as possible and to achieve maximum resolution in the analyse, the chamber volume shall be kept as small as possible.
The process is basically a gas chromatography where a chamber with a light path is added in the end of the column so the gas passes through the chamber and absorbs light with a spectrum that is related to the gas.
The remaining lights then passes into a spectrograph and further on to a light sensitive sectioned array preferably a CCD, Charge Coupled Device, so the spatial light components hits individual light sensitive elements enabling spatial detection of the light and thereby allows identification of the substance to be analysed.
Light is directed in to the spectrograph trough a passage that can be a window made out of a photon transparent material that allow passage of the required wavelengths.
In order to have maximum number of photons to reach the light sensitive element it is important to use windows separating the spectrograph from the gas path in material that has very high transparency, particular in the low wavelength range.
Materials used in such windows can be made of MgF2 or material with similar optical properties with the drawback like of being sensitive to rapid
degradation and consequently loss of transparency. Any physical window acts as a filter of passing photons in particular for short wavelength photons. It is also important to keep the spectrograph, its dispersive element and photon sensitive array clean from contamination like particles and residuals from gases, like sublimated matter from gas in order to keep the functionality of the spectrograph.
A physical window has to be cleaned or replaced regularly due to
contamination. It would be an advantage not to use a physical window but without a device that will prevent gas or particles to enter through the slit of the spectrograph it will otherwise rapidly be contaminated and loose its functionality. Therefore an improvement over such devices is desirable.
SUMMARY OF THE INVENTION
An object of the present invention is to eliminate at least one of the drawbacks mentioned above, which is achieved by assigning to the characteristics according to claim 1- 8.
According to a first aspect of the invention, is that the light entrance to the spectrograph is not provided with a physical solid barrier like a physical window, but prevention of gas to be analysed to enter the spectrograph is made by flow of inert gas like nitrogen or other gases out from the
spectrograph trough light entrance slit of the spectrograph.
Different pressure at the different locations directs the flow of gas in a desired way from locations with higher pressure to locations with lower pressure. If the gas pressure in the spectrograph is kept higher than outside, the gas flow from the spectrograph passes out through the slit and there will be an efficient barrier against intrusion of gas, still with the ability for short wavelength light to pass through from outside into the spectrograph..
According to a second aspect of the invention the light entrance to the spectrograph is not provided with a physical solid barrier like a physical window, but preventing the amount of gas to be analysed to enter the spectrograph can be made by having the entrance slit so small that the undesired entrance of gas from outside into the spectrograph is of minor importance for the function.
According to a third aspect of the invention, there is no physical window that requires cleaning or replacement due to contamination. The solution will by that reduce operating cost and increase up time and general functionality.
According to a forth aspect of the invention it allows spectral resolution down to below 120nm wave length to be analysed.
BRIEF DESCRIPTION OF THE DRAWINGS
In order to explain the invention, a number of embodiments of the invention will be described below with reference to the drawings, in which:
Fig. 1 shows schematically a device in accordance with a first embodiment of the invention, and
Fig. 2 shows schematically a device in accordance with a second
embodiment of the invention
Same reference numerals have been used to indicate the same parts in the figures to increase the readability of the description and for the sake of clarity. The figures are not made to scale, and the relative dimensions of the illustrated objects may be disproportional.
DETAILED DESCRIPTION
The invention relates to a method of increasing the transparency of very short wavelength photons in GC-UV applications.
Fig. 1 shows schematically a spectrometer (9) comprising a spectrograph (8) with a dispersive element (1 ) with light beams (3, 5) passing through a small slit (7) and reflects at the dispersive element (1 ) and hits a light sensitive element (2) like a CCD (2). A gas supplying means (not shown) is provided for producing gas flows (4) into the spectrograph and then out of the spectrograph trough a slit (7). The pressure of the gas decline from where it enters (4) the spectrograph to where then the gas exit from the spectrograph trough the slit (7). The drop of pressure over the slit (7) creates a velocity of the gas that prevents gas or particles to enter through the slit (7) in the reverse direction.
As long as the pressure is higher at the point where the gas enters the spectrometer than the point where it leaves the spectrometer there will be a gas flow where the gas has a velocity preventing gas or particles to enter the spectrograph.
As the spectrograph - spectrometer does not comprise a physical window, but only a dynamic gas flow that does not filter any of the light (5) that enters through the slit (7) the full spectrum of incoming lights (5) will enter the spectrograph - spectrometer.
According to a second aspect of the invention there is no gas flow (4) into the spectrograph, but undesired flow of gas to be analysed through the slit (7) is kept at a minimum by minimizing the size of the slit.
Fig. 2 shows schematically a spectrometer (9) comprising a spectrograph (8) with a dispersive element (1 ) with light beams (3, 5) passing through a slit (7) and reflects at the dispersive element (1 ) and hits a light sensitive element (2) like a CCD (2). The slit (7) is so small that the flow of gas from outside the spectrograph into the same is so small that it will only marginally affect the function of the spectrograph and spectrometer.
Definitions: A spectrograph is consisting of a slit (7) where light enters, a dispersive element that reflects the fractioned light. A spectrometer is a spectrograph that has a photon collecting device (2) to collect the fractioned light (10) for read out and measurement of spectra. The Photon collecting device can be a CCD - Charge Collecting Device (2). Additionally, although individual features may be included in different embodiments, these may possibly be combined in other ways, and the inclusion in different embodiments does not imply that a combination of features is not feasible. In addition, singular references do not exclude a plurality. The terms "a", "an" does not preclude a plurality. Reference signs in the claims are provided merely as a clarifying example and shall not be construed as limiting the scope of the claims in any way.

Claims

1 . A method for obtain photonic signal levels and spatial resolution from samples in gas phase of substances by a first step selection by time by gas chromatography and by a second step by absorption of photons by UV light that passes a chamber with the gas for identification and quantification of substances, characterized by directing light through a light entrance slit of a following spectrograph that has no physical window or windows in the light path.
2. A method as claimed in claim 1 also including providing a gas flow through the light entrance slit that has an opposite direction to the light, so as to prevent a gas flow or particles to enter said spectrograph.
3. A method as claimed in claim 2, also including providing a gas pressure inside said spectrograph that is at least 1 bar higher in relation to outside the spectrograph.
4. A method as claimed in claim 2 or claim 3, also including directing an incoming gas flow through an inlet arrangement and directing an outlet flow through a spectrograph dispersive slit.
5. An apparatus for obtaining photonic signal levels and spatial resolution from samples in gas phase of substances by absorption of photons by UV light that passes a chamber with the gas for identification and quantification of substances, characterized by an open light entrance of a following spectrograph without physical window or windows in the light path.
6. An apparatus as claimed in claim 5, comprising a gas supplying means providing a gas flow through the light entrance slit that has an opposite direction as compared to the light.
7. An apparatus as claimed in claim 5 or claim 6, wherein means are provided for obtaining photonic signal levels and spatial resolution from UV light down to120nm of wavelength.
8. An apparatus as claimed in claim 6 or claim 7, wherein said gas supplying means produces a gas pressure inside said following spectrograph is at least 1 bar higher than outside the said spectrograph.
9. An apparatus as claimed in any of claims 6-8, wherein an inlet
arrangement is provided for incoming gas and a spectrograph dispersive slit is provided for an outlet flow.
PCT/SE2011/050970 2010-08-01 2011-07-26 Spectrograph for short wavelength detection in gas chromatography - uv detection WO2012018299A1 (en)

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US36973410P 2010-08-01 2010-08-01
US61/369,734 2010-08-01

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9116158B2 (en) 2012-10-18 2015-08-25 Vuv Analytics, Inc. Vacuum ultraviolet absorption spectroscopy system and method
US10677767B2 (en) 2018-06-12 2020-06-09 Vuv Analytics, Inc. Vacuum ultraviolet absorption spectroscopy system and method

Citations (2)

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US4441815A (en) * 1981-03-31 1984-04-10 Anritsu Electric Company Limited Self-modulating spectrometer
DE10302207A1 (en) * 2003-01-20 2004-07-29 Krieg, Gunther, Prof. Dr.-Ing. Highly sensitive, selective measurement of minimal gas quantities using absorption or fluorescence spectroscopy, with a measurement cell in the form of a miniaturized hollow optical wave-guide

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4441815A (en) * 1981-03-31 1984-04-10 Anritsu Electric Company Limited Self-modulating spectrometer
DE10302207A1 (en) * 2003-01-20 2004-07-29 Krieg, Gunther, Prof. Dr.-Ing. Highly sensitive, selective measurement of minimal gas quantities using absorption or fluorescence spectroscopy, with a measurement cell in the form of a miniaturized hollow optical wave-guide

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
ANTHONY C. GILBY: "Optical design of a new photodiode array absorbance detector for high-performance liquid chromatography", PROCEEDINGS OF SPIE, vol. 1681, 1 January 1992 (1992-01-01), pages 54 - 66, XP055009889, ISSN: 0277-786X, DOI: 10.1117/12.137760 *
LAGESSON-ANDRASKO L ET AL: "THE USE OF GAS-PHASE UV SPECTRA IN THE 168-330-NM WAVELENGTH REGIONFOR ANALYTICAL PURPOSES. 1. QUALITATIVE MEASUREMENTS", ANALYTICAL CHEMISTRY, AMERICAN CHEMICAL SOCIETY, US, vol. 70, no. 5, 1 March 1998 (1998-03-01), pages 819 - 826, XP000750430, ISSN: 0003-2700, DOI: 10.1021/AC971009V *
ROBERT HODYSS ET AL: "Multidimensional Detection of Nitroorganic Explosives by Gas Chromatography-Pyrolysis-Ultraviolet Detection", ANALYTICAL CHEMISTRY, vol. 77, no. 11, 1 June 2005 (2005-06-01), pages 3607 - 3610, XP055010034, ISSN: 0003-2700, DOI: 10.1021/ac050308e *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9116158B2 (en) 2012-10-18 2015-08-25 Vuv Analytics, Inc. Vacuum ultraviolet absorption spectroscopy system and method
US9465015B2 (en) 2012-10-18 2016-10-11 Vuv Analytics, Inc. Vacuum ultraviolet absorption spectroscopy system and method
US9696286B2 (en) 2012-10-18 2017-07-04 Vuv Analytics, Inc. Vacuum ultraviolet absorption spectroscopy system and method
US9891197B2 (en) 2012-10-18 2018-02-13 Vuv Analytics, Inc. Vacuum ultraviolet absorption spectroscopy system and method
US9976996B2 (en) 2012-10-18 2018-05-22 Vuv Analytics, Inc. Vacuum ultraviolet absorption spectroscopy system and method
US10338040B2 (en) 2012-10-18 2019-07-02 Vuv Analytics, Inc. Vacuum ultraviolet absorption spectroscopy system and method
US10641749B2 (en) 2012-10-18 2020-05-05 Vuv Analytics, Inc. Vacuum ultraviolet absorption spectroscopy system and method
US10677767B2 (en) 2018-06-12 2020-06-09 Vuv Analytics, Inc. Vacuum ultraviolet absorption spectroscopy system and method

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