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WO1998005956A1 - Detecteur a ionisation pour la chromatographie en phase gazeuse - Google Patents

Detecteur a ionisation pour la chromatographie en phase gazeuse Download PDF

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Publication number
WO1998005956A1
WO1998005956A1 PCT/DE1996/001478 DE9601478W WO9805956A1 WO 1998005956 A1 WO1998005956 A1 WO 1998005956A1 DE 9601478 W DE9601478 W DE 9601478W WO 9805956 A1 WO9805956 A1 WO 9805956A1
Authority
WO
WIPO (PCT)
Prior art keywords
detector
ionization detector
gas
heated
ionization
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/DE1996/001478
Other languages
German (de)
English (en)
Inventor
Michael Beckmann
Hans-Herrmann RÜTTINGER
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Preussag Wasser und Rohrtechnik GmbH
Original Assignee
Preussag Wasser und Rohrtechnik GmbH
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
Priority to DE19502285A priority Critical patent/DE19502285C2/de
Application filed by Preussag Wasser und Rohrtechnik GmbH filed Critical Preussag Wasser und Rohrtechnik GmbH
Priority to PCT/DE1996/001478 priority patent/WO1998005956A1/fr
Publication of WO1998005956A1 publication Critical patent/WO1998005956A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

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
    • G01N30/64—Electrical detectors
    • G01N30/68—Flame ionisation detectors
    • 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
    • G01N30/64—Electrical detectors
    • G01N2030/647—Electrical detectors surface ionisation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/626—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas

Definitions

  • the majority of the detectors used in GC work on the principle of charge transport in an electrical field. With the help of different techniques (e.g. flames, photons, ß-radiation) ions are generated, which are registered directly or indirectly.
  • different techniques e.g. flames, photons, ß-radiation
  • Flame ionization detectors burn the substances (eluate) eluting from a chromatographic separation column in a hydrogen / air diffusion flame above a nozzle.
  • the ionization yield in the FID is very low.
  • the standard sensitivity of approx. 0.016 A * s / g carbon shows that only one ion pair is formed from approximately 500,000 carbon atoms.
  • FID Flameless ionization detectors
  • the thermionic emitter consists of ceramic material with various alkali salt additives, which are used with the sample components
  • SPARE 2 BLADE React ion formation and be consumed in the process.
  • the response and sensitivity of these detectors depend on the amount of reactive ions present and therefore changes over the course of the detector's operating time.
  • An electrically heated ion emitter 4> is used as an electrically heated ion emitter 4> .
  • This version (thermionic detector, TID) is characterized in that the energy required for ion emission is no longer provided by a hydrogen flame. Nevertheless, these detectors require a low and constant volume flow of hydrogen to form a specific reaction zone.
  • the problem stated in the invention is based on the problem of creating a detector which, with a high ion yield, has a response behavior and sensitivity which is independent of consuming reactive ions and which enables hydrogen-free operation.
  • the detector is equipped with a heated nozzle, preferably made of ceramic material.
  • a heated nozzle preferably made of ceramic material.
  • Alumina base The materials should preferably have volume resistivities of> 10 14 ⁇ (20 ° C).
  • the heating windings should be provided with a ceramic layer to protect them from oxidation and / or aggressive media.
  • materials doped with alkali and / or alkaline earth salts are also suitable as ceramic materials.
  • the detector consists of two parts, the detector base (A) and the detector head (B).
  • the detector base and head are preferably made of an iron / nickel / cobalt alloy.
  • the nozzle (C) is formed from a ceramic tube (e.g. made of Rubalit ® 717), which is embedded in the metallic screw connection (N) with the aid of a ceramic adhesive and is thus gas-tightly connected to the detector base.
  • the ceramic tube is wrapped with a heating wire (H).
  • the heating wire is surrounded by a thin ceramic layer or another thin ceramic tube (J).
  • the detector base contains holes that are provided for the supply of the electrical heating current (D) and for the supply of reactive gases (E).
  • the detector head contains a collector electrode (F) which is electrically insulated from other components of the detector and is conductively connected to a shielded measurement signal lead (G).

Landscapes

  • 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)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

L'invention concerne un détecteur à ionisation comportant un émetteur thermoionique. Le mode de réponse et la sensibilité des détecteurs de la technique antérieure utilisés avec ce type d'émetteur dépendent de la quantité d'ions réactifs présents et varient donc au cours de la période de fonctionnement. Pour éviter ce phénomène, il est prévu d'équiper le détecteur d'une buse chauffante dans laquelle les substances organiques à détecter sont mises en contact sans flamme avec un gaz réactif. La température de la buse peut atteindre jusqu'à 1200 °C.
PCT/DE1996/001478 1995-01-26 1996-08-07 Detecteur a ionisation pour la chromatographie en phase gazeuse Ceased WO1998005956A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
DE19502285A DE19502285C2 (de) 1995-01-26 1995-01-26 Ionisationsdetektor für die Gaschromatographie
PCT/DE1996/001478 WO1998005956A1 (fr) 1995-01-26 1996-08-07 Detecteur a ionisation pour la chromatographie en phase gazeuse

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19502285A DE19502285C2 (de) 1995-01-26 1995-01-26 Ionisationsdetektor für die Gaschromatographie
PCT/DE1996/001478 WO1998005956A1 (fr) 1995-01-26 1996-08-07 Detecteur a ionisation pour la chromatographie en phase gazeuse

Publications (1)

Publication Number Publication Date
WO1998005956A1 true WO1998005956A1 (fr) 1998-02-12

Family

ID=25962842

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/DE1996/001478 Ceased WO1998005956A1 (fr) 1995-01-26 1996-08-07 Detecteur a ionisation pour la chromatographie en phase gazeuse

Country Status (2)

Country Link
DE (1) DE19502285C2 (fr)
WO (1) WO1998005956A1 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102539591B (zh) * 2011-12-31 2014-04-16 聚光科技(杭州)股份有限公司 一种小型化氢火焰离子化检测装置
DE102018212089A1 (de) * 2018-07-19 2020-01-23 Hochschule Karlsruhe Sensorvorrichtung und ein Verfahren zur Erfassung eines Kohlenwasserstoff-Anteils

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3423181A (en) * 1966-06-06 1969-01-21 Varian Associates Thermionic detector for gas chromatography
US3589869A (en) * 1969-02-17 1971-06-29 Varian Associates Chemical-ionization detection method and apparatus
US3607096A (en) * 1969-06-25 1971-09-21 Charles H Hartmann Alkali flame ionization detector having cap means for changing the gas flow pattern
DE2907222A1 (de) * 1978-02-28 1980-01-10 Varian Associates Verfahren und vorrichtung zur analyse einer probe
GB2037066A (en) * 1978-10-09 1980-07-02 Simpson C Flame ionisation detector and method of use thereof
DE3835081A1 (de) * 1985-06-11 1989-04-27 Inst Elektroniki Im U A Arifov Verfahren und einrichtung zur analyse organischer verbindungen mittels der chromatographie
US4999162A (en) * 1988-08-26 1991-03-12 Varian Associates, Inc. High temperature flame jet for gas chromatography
US5019517A (en) * 1988-04-15 1991-05-28 Coulson Dale M System, detector and method for trace gases
US5521098A (en) * 1994-07-27 1996-05-28 Hewlett-Packard Company Thermionic ionization detector with flow-through thermionic source

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3585003A (en) * 1967-04-06 1971-06-15 Varian Associates Ionization detector for gas chromatography
US4182740A (en) * 1976-03-01 1980-01-08 Varian Associates, Inc. Flame ionization detector

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3423181A (en) * 1966-06-06 1969-01-21 Varian Associates Thermionic detector for gas chromatography
US3589869A (en) * 1969-02-17 1971-06-29 Varian Associates Chemical-ionization detection method and apparatus
US3607096A (en) * 1969-06-25 1971-09-21 Charles H Hartmann Alkali flame ionization detector having cap means for changing the gas flow pattern
DE2907222A1 (de) * 1978-02-28 1980-01-10 Varian Associates Verfahren und vorrichtung zur analyse einer probe
GB2037066A (en) * 1978-10-09 1980-07-02 Simpson C Flame ionisation detector and method of use thereof
DE3835081A1 (de) * 1985-06-11 1989-04-27 Inst Elektroniki Im U A Arifov Verfahren und einrichtung zur analyse organischer verbindungen mittels der chromatographie
US5019517A (en) * 1988-04-15 1991-05-28 Coulson Dale M System, detector and method for trace gases
US4999162A (en) * 1988-08-26 1991-03-12 Varian Associates, Inc. High temperature flame jet for gas chromatography
US5521098A (en) * 1994-07-27 1996-05-28 Hewlett-Packard Company Thermionic ionization detector with flow-through thermionic source

Also Published As

Publication number Publication date
DE19502285A1 (de) 1996-08-08
DE19502285C2 (de) 1996-11-21

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