WO2012018298A1 - Spectrophotomètre uv pour identifier et détecter des composés élués après séparation chromatographique en phase gazeuse - Google Patents

Spectrophotomètre uv pour identifier et détecter des composés élués après séparation chromatographique en phase gazeuse Download PDF

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Publication number
WO2012018298A1
WO2012018298A1 PCT/SE2011/050969 SE2011050969W WO2012018298A1 WO 2012018298 A1 WO2012018298 A1 WO 2012018298A1 SE 2011050969 W SE2011050969 W SE 2011050969W WO 2012018298 A1 WO2012018298 A1 WO 2012018298A1
Authority
WO
WIPO (PCT)
Prior art keywords
light
gas flow
gas
arrangement according
detector arrangement
Prior art date
Application number
PCT/SE2011/050969
Other languages
English (en)
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 WO2012018298A1 publication Critical patent/WO2012018298A1/fr

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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
    • 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
    • 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
    • G01J3/0205—Optical elements not provided otherwise, e.g. optical manifolds, diffusers, windows
    • G01J3/0208—Optical elements not provided otherwise, e.g. optical manifolds, diffusers, windows using focussing or collimating elements, e.g. lenses or mirrors; performing aberration correction
    • 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
    • G01J3/28—Investigating the spectrum
    • 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
    • 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

  • UV spectrophotometer for identification and detection of eluting compounds from gas chromatographic separations.
  • the present invention relates to spectrophotometric measurements of vapors and gases in vacuum, far and UVC wavelength region (120 - 400 nm)
  • the invention relates Gas Chromatography, GC - Ultraviolet absorption, UV - spectroscopy, GC-UV, to detect and identify, analyse of gases and liquid 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 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 f.ex. stress.
  • Substances can be such as nitrogen oxide, urea, acetone, isoprene, carbon disulfide coming from diseases like gastric ulcers, asthma, diabetes, psychiatric disorders, drug abuse, stress conditions and intoxications, etc.
  • UV light absorption in the liquid phase is widely used in various types of analyzers.
  • the light source used is usually deuterium lamps.
  • a flow cell with transparent windows, which usually consists of fused silica are employed.
  • the detector part in these arrangements is usually a spectrograph combined with a photo diode array element (PDA).
  • PDA photo diode array element
  • UV light absorption in the vapour/gas phase in combination with gas chromatographic separation are only described in a few cases. The principal is of these measurements is similar to those in the liquid phase but there are a number important and significant differences.
  • the wavelength range accessible in the vapour/gas is not limited by any solvent cut off which opens up for recordings at short wavelengths in the vacuum to far UV region 140 - 200 were very important and conclusive spectral information is present.
  • the optical elements suitable for measuring in this wavelength regions are window materials consisting of magnesium fluoride (MgF2) with transmittance of 50 - 95 % from 120 - 400 nm, sapphire with transmittance of 70 - 83 % from 150 - 400 nm and synthetic fused silica with transmittance of 70 - 80 % from 165 - 400 nm.
  • the mirror suitable for these measurements are Al mirrors which have a reflectance of 80 - 90 from 145 - 400 nm.
  • the measurements in this wavelength region also implies that recordings are performed in an inert atmosphere were water vapour and oxygen are carefully removed. This atmosphere could be nitrogen (which absorbs light at wavelengths below 120 nm) or permanent / noble gases like helium, argon or hydrogen.
  • the detector part in this arrangement is a spectrograph combined with preferably a back thinned type of CCD element.
  • This type of detector ship has a considerably more favourable quantum efficiency and response at shorter wavelengths.
  • the characteristics of the invention are illustrated in the enclosed figure.
  • the embodiment shown comprises a lamp emitting the light beam to a parabolic mirror which guides and focus the light into a gas flow cell where the flow of compounds eluting from an external gas chromatograph passes through.
  • the light output from the gas flow cell is collected at the outlet and further guided to the entrance slit of a spectrometer to measure spectra appearing in the light beam.
  • the conventional carrier gases for gas chromatography are nitrogen, helium and hydrogen which are all transparent in the wavelength range of interest.
  • the lamp compartment including the parabolic mirror and the spectrograph compartment are all flushed with dry nitrogen in order to prevent any absorption from water vapour and oxygen.
  • the parabolic mirror can be tilted, so that the focus that normally by measurement of a substance is at the light entrance to the spectrograph, is moved to eliminate the ability for the light to enter the spectrograph enabling dark calibration of the light sensitive elements like CCD.
  • the objects of the present invention are to achieve functionality by assigning to the characteristics according to claim 1- 10.
  • a device that has the capability to analyse and identify substances in gas phase by absorption of UV light penetrating the gas with a spectral distribution of the light energy that corresponds to, identifies and quantifies the substance.
  • the absorption of UV light takes place in a tubular shaped arrangement where light penetrates along the axis of the device.
  • the light that penetrates the substance in gas phase is focused to the light pipe by identification and can be switched on and off by moving the focus from the light pipe.
  • a fifth aspect of the invention it allows the light to be in reverse direction relative the gas flow.
  • the embodiment shown in Figure 1 comprises:
  • a body (1 ) being temperature regulated up to 300 °C,
  • a preferably quartz capillary (2) typically, but not limited to10 - 300 mm length with aluminum or other high UV reflective coating at inside or the outside and having an internal diameter of 0.1 - 10 mm ("light pipe").
  • MCF2 magnesium fluoride
  • a parabolic Al mirror (4) (freshly MGF2 coated), serving by measurement of a substance, by directing the light from the lamp (3) to the quartz capillary (2) through a window (5) and also serving as a shutter by dark calibration of the spectrometer by redirecting the light by rotation so that the focus will be away from the window (5) and the quarts capillary (2) comprising such as;, a MGF2 (5) alternatively a sapphire window
  • GC-VUV gas chromatographic
  • the magnesium fluoride (MGF2) can be other materials like sapphire or other material with sufficient optical transparency at wavelengths down below 120nm.
  • a light pipe is a tubular shaped device where substances in gas phase passes, penetrated by light and where the light is fully or partially absorbed by the gas molecules with a spectrum that relates to the substance.
  • a spectrograph is consisting of a slit where light enters, a dispersive element that reflects the fractioned light.
  • a spectrometer is a spectrograph that has a photon collecting device to collect the fractioned light for read out and measurement of spectra.
  • the Photon collecting device can be a CCD - Charge 5 Collecting Device.

Landscapes

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

Abstract

L'invention concerne un détecteur UV de spectrographie pour chromatographie en phase gazeuse, qui permet d'augmenter efficacement le flux de photons à travers le spectrographe vers un ou plusieurs éléments photosensibles, tout en restant fonctionnel.
PCT/SE2011/050969 2010-08-01 2011-07-26 Spectrophotomètre uv pour identifier et détecter des composés élués après séparation chromatographique en phase gazeuse WO2012018298A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US36973810P 2010-08-01 2010-08-01
US61/369,738 2010-08-01

Publications (1)

Publication Number Publication Date
WO2012018298A1 true WO2012018298A1 (fr) 2012-02-09

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014062419A1 (fr) * 2012-10-18 2014-04-24 Vuv Analytics, Inc. Système de spectroscopie d'absorption dans l'ultraviolet sous vide et procédé associé
WO2014128180A1 (fr) * 2013-02-20 2014-08-28 Chromalytica Ab Diode électroluminescente ultraviolette utilisée comme source de lumière en chromatographie en phase gazeuse-spectrophotométrie d'absorption uv
WO2014170384A1 (fr) * 2013-04-17 2014-10-23 Chromalytica Ab Unité de désorption thermique directe liée à une chromatographie en phase gazeuse - détection en ultraviolet (uv)
US10677767B2 (en) 2018-06-12 2020-06-09 Vuv Analytics, Inc. Vacuum ultraviolet absorption spectroscopy system and method
CN115266640A (zh) * 2022-08-05 2022-11-01 东北大学 一种基于空芯光纤微腔的自参考气体吸收光谱检测装置及方法

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DE3615259A1 (de) * 1986-05-06 1987-11-12 Krieg Gunther Verfahren und system zur kontinuierlichen bestimmung der konzentrationen von molekuehlverbindungen in fluessigkeiten und gasen
EP0539021A1 (fr) * 1991-10-22 1993-04-28 Puritan-Bennett Corporation Commutateur optique de voies de signaux
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US20020149767A1 (en) * 2001-04-16 2002-10-17 Eiji Ishikawa Variable slit width device for spectroscope
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US20070161876A1 (en) * 2005-11-18 2007-07-12 Spectrx, Inc. Method and apparatus for rapid detection and diagnosis of tissue abnormalities
US20090015820A1 (en) * 2006-10-26 2009-01-15 Thomas Bohe Method and apparatus for the analysis of foreign gas phase in containers

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DE3615259A1 (de) * 1986-05-06 1987-11-12 Krieg Gunther Verfahren und system zur kontinuierlichen bestimmung der konzentrationen von molekuehlverbindungen in fluessigkeiten und gasen
EP0539021A1 (fr) * 1991-10-22 1993-04-28 Puritan-Bennett Corporation Commutateur optique de voies de signaux
US6307204B1 (en) * 1997-11-14 2001-10-23 Jasco Corporation UV detector for liquid chromatography
US20010010747A1 (en) * 1999-02-10 2001-08-02 Dourdeville Theodore A. Flow cell , analyte measurement apparatus and methods related thereto
US20020149767A1 (en) * 2001-04-16 2002-10-17 Eiji Ishikawa Variable slit width device for spectroscope
DE10302207A1 (de) * 2003-01-20 2004-07-29 Krieg, Gunther, Prof. Dr.-Ing. Verfahren und vorrichtung zur Messung von Gasen bei kleinsten Volumina und höchster Empfindlichkeit
US20070161876A1 (en) * 2005-11-18 2007-07-12 Spectrx, Inc. Method and apparatus for rapid detection and diagnosis of tissue abnormalities
US20090015820A1 (en) * 2006-10-26 2009-01-15 Thomas Bohe Method and apparatus for the analysis of foreign gas phase in containers

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DIMITRIS G. HATZINIKOLAOU ET AL: "Analysis of the Gas Phase of Cigarette Smoke by Gas Chromatography Coupled with UV-Diode Array Detection", ANALYTICAL CHEMISTRY, vol. 78, no. 13, 1 July 2006 (2006-07-01), pages 4509 - 4516, XP055009029, ISSN: 0003-2700, DOI: 10.1021/ac052004y *
H.S. ECKHARDT ET AL: "Fiber-optic detection device for GC-UV", PROCEEDINGS OF SPIE, vol. 6433, 1 January 2007 (2007-01-01), pages 64330D-1 - 64330D-7, XP055009031, ISSN: 0277-786X, DOI: 10.1117/12.717694 *
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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9696286B2 (en) 2012-10-18 2017-07-04 Vuv Analytics, Inc. Vacuum ultraviolet absorption spectroscopy system and method
CN104736989A (zh) * 2012-10-18 2015-06-24 Vuv分析公司 真空紫外吸收光谱系统和方法
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
WO2014062419A1 (fr) * 2012-10-18 2014-04-24 Vuv Analytics, Inc. Système de spectroscopie d'absorption dans l'ultraviolet sous vide et procédé associé
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
WO2014128180A1 (fr) * 2013-02-20 2014-08-28 Chromalytica Ab Diode électroluminescente ultraviolette utilisée comme source de lumière en chromatographie en phase gazeuse-spectrophotométrie d'absorption uv
WO2014170384A1 (fr) * 2013-04-17 2014-10-23 Chromalytica Ab Unité de désorption thermique directe liée à une chromatographie en phase gazeuse - détection en ultraviolet (uv)
US10677767B2 (en) 2018-06-12 2020-06-09 Vuv Analytics, Inc. Vacuum ultraviolet absorption spectroscopy system and method
CN115266640A (zh) * 2022-08-05 2022-11-01 东北大学 一种基于空芯光纤微腔的自参考气体吸收光谱检测装置及方法

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